Dyeing method of cellulose-based fiber product

Abstract

To provide a dyeing method of a cellulose-based fiber fabric which reduces CO2 emission by shortening a dyeing time, simplifies dyeing operation, and can obtain a uniform dyed material having high color fastness and no color evenness.SOLUTION: A dyeing method of a cellulose-based fiber or a fiber product containing a cellulose fiber includes the steps of: supplying water in a first temperature region of 5°C or higher and lower than 30°C or water in a second temperature region of 30°C or higher and lower than 40°C, to a dyeing bath, and charging a cellulose-based fiber of a fiber product containing a cellulose-based fiber; a temperature raising step of raising the temperature up to the second temperature region of 30°C or higher and lower than 40°C from the first temperature region, and raising the temperature up to a third temperature region of 40°C or higher and 70°C or lower from the second temperature region; keeping a predetermined period temperature in the third temperature region; charging a reaction dye at a temperature equal to or higher than the first temperature region; and dividing and charging a mixture of inorganic salts and an alkali agent three or more times separately from the step of charging the reaction dye at a temperature equal to or higher than the second temperature region.SELECTED DRAWING: Figure 2

Description

[Technical field]

[0001] The present invention relates to a method for dyeing cellulosic fibers or textile products containing cellulosic fibers with reactive dyes. [Background technology]

[0002] In industrial exhaust dyeing, when reactive dyes are used, inorganic salts and alkaline agents are added to the dye bath together with the reactive dye, and exhaust dyeing of the reactive dye is carried out. The presence of inorganic salts is necessary to promote the absorption of the dye into the cellulose fibers, while the alkaline agent is necessary to fix the reactive dye to the cellulose fibers. It is generally known that the addition of inorganic salts and alkaline agents to the dye bath is an important factor for obtaining uniform dyed products. In conventional dyeing processes, inorganic salts are added in appropriate portions to the dye bath in which water, fabric, and dye are uniformly dispersed, and after the addition of inorganic salts is completed, alkaline agents are also added in appropriate portions.

[0003] However, with the conventional techniques, it takes a long time to obtain uniform dyed products with high color fastness and no color unevenness, and a lot of electricity is consumed to operate the dyeing machine and steam to maintain temperature, resulting in a large amount of CO 2 There is a problem of increased emissions.

[0004] The following Patent Document 1 proposes an exhaustion dyeing method for shortening the dyeing time, in which a reactive dye having a specific molecular structure is used and this dye is added together with inorganic salts and an alkaline agent. However, in the method of adding inorganic salts and an alkaline agent at once, since inorganic salts have a property of being difficult to dissolve, it takes time to dissolve the inorganic salts, and the workability becomes complicated. Furthermore, adding inorganic salts at once causes a phenomenon in which the dye is instantly absorbed by the cellulose fibers, and from the viewpoint of obtaining a uniform dyed product, a sufficient dyeing result is not obtained.

[0005] Furthermore, the following Patent Document 2 proposes a method of adding an inorganic salt and an alkaline agent in separate portions, in which the inorganic salt and the alkaline agent are optimally added in small amounts per unit time according to a linear function or a positive or negative exponential, logarithmic, or power function. However, in the technology of Patent Document 2, although the inorganic salt and the alkaline agent are optimally added in infinite steps using special dedicated equipment, in order to determine the optimal addition rate of the inorganic salt and the alkaline agent, a series of exhaust dyeing tests must be performed in advance and calculated from the addition function of the isothermal exhaust curve using a computer program, and further, if the simultaneous addition rate of the inorganic salt and the alkaline agent changes according to a non-linear addition function, this function must be determined using a data processing unit (e.g., a personal computer). In other words, there was a problem that very complicated and cumbersome work was required until the addition rate was determined, and mathematical knowledge was also required. Furthermore, in order to realize the addition rate obtained by calculation, it is impossible to do it manually, so a dedicated equipment is required to add the dye bath while measuring in real time during the dyeing process, and since it requires capital investment, it is not easy to implement. This is particularly true in developing countries.

[0006] Furthermore, the following Patent Document 3 proposes a method of adding an inorganic salt and an alkaline agent in portions after mixing them, in which the inorganic salt and the alkaline agent are added quantitatively and continuously, as shown by any of three specific curves. However, in the technology of Patent Document 3, in order to realize the addition rate shown in any of the three specific curves, it is impossible to do it manually, so a dedicated facility for adding the dye into the dye bath is required, which requires capital investment, and therefore it is not easy to implement, especially in developing countries.

[0007] In this way, shortening the staining time can reduce the 2 At present, there is no method for dyeing cellulosic fiber fabrics that can reduce emissions, simplify the dyeing operation, and give uniformly dyed products with high color fastness and no color unevenness. [Prior art documents] [Patent documents]

[0008] [Patent Document 1] Japanese Patent Application Publication No. 63-211379 [Patent Document 2] Japanese Patent Application Publication No. 60-259687 [Patent Document 3] Japanese Patent Application Publication No. 01-118680 [Non-patent literature]

[0009] [Non-Patent Document 1] Reference Material 2: List of formulas and emission factors for calculating greenhouse gas emissions (https: / / www.env.go.jp / earth / ondanka / suishin_g / 3rd_edition / ref2.pdf) Summary of the Invention [Problem to be solved by the invention]

[0010] In view of the above-mentioned state of the art, the problem to be solved by the present invention is to reduce the dyeing time and to 2 The present invention provides a novel method for dyeing cellulosic fiber fabrics, which simplifies the dyeing operation while reducing emissions and enables the production of uniformly dyed products with high color fastness and no color unevenness. [Means for solving the problem]

[0011] As a result of intensive research and repeated experiments to solve the above problems, the inventors unexpectedly discovered that by dividing the addition method of the mixture of inorganic salts and alkaline agents into predetermined number of additions and optimizing the temperature of the dyeing solution and the timing of addition, it is possible to obtain uniformly dyed products having high dyeing fastness and no color unevenness without using the above-mentioned special dedicated equipment, and thus completed the present invention.

[0012] That is, the present invention is as follows. [1] A method for dyeing cellulosic fibers or textile products containing cellulosic fibers, comprising the following steps: supplying water in a first temperature range of 5° C. or more and less than 30° C., or in a second temperature range of 30° C. or more and less than 40° C., and simultaneously introducing a textile product of or containing cellulosic fibers into the dyebath, regardless of whether the introduction of water occurs before or after the introduction of water; a temperature increasing step of increasing the temperature from the first temperature region to a second temperature region of 30° C. or more and less than 40° C., and from the second temperature region to a third temperature region of 40° C. or more and 70° C. or less, or from the second temperature region to a third temperature region of 40° C. or more and 70° C. or less; maintaining the third temperature within the third temperature range for a predetermined period of time; dosing a reactive dye at a temperature equal to or greater than the first temperature range; and a step of adding a mixture of an inorganic salt and an alkali agent in three or more portions at a temperature equal to or higher than the second temperature region, separately from the step of adding the reactive dye; A dyeing method comprising the steps of: [2] The following process: maintaining the temperature within the second temperature zone for a predetermined period of time; The dyeing method according to [1] above, further comprising: [3] The dyeing method according to [1], wherein all of the mixture of the inorganic salt and the alkaline agent is added in portions within the third temperature zone. [4] The dyeing method according to [2], wherein the mixture of the inorganic salt and the alkaline agent is added in whole in portions within the second temperature region. [5] The divided addition is carried out three or more times and five or less times. When the total amount of the mixture of the inorganic salt and the alkaline agent is T(g), the amount added in the first stage is A(g), and the amount added in the second stage is B(g), the following formulas (1) to (3) are satisfied: 1 / 20×T≦A≦5 / 20×T…Formula (1) 1 / 20×T≦B≦7 / 20×T…Formula (2) A≦B…Formula (3) The dyeing method according to any one of the above [1] to [4], [6] The dyeing method according to any one of [1] to [5] above, wherein the total time period from the water supply to the end of the third temperature holding step is 100 minutes or less. [7] The dyeing method according to [6], wherein the total time period is 80 minutes or less. [8] The dyeing method according to any one of [1] to [7], wherein a dyeing reaction time period from the final stage of the divided addition to the end of the third temperature holding step is 20 minutes or more and 50 minutes or less. [9] The dyeing method according to [8], wherein the dyeing reaction time period is 40 minutes or more.

[10] The dyeing method according to any one of [1] to [9], wherein the third temperature is maintained at 60° C. or lower.

[11] The dyeing method according to any one of [1] to

[10] above, wherein the time interval between the divided additions is 5 minutes to 17 minutes. Effect of the Invention

[0013] According to the dyeing method of the present invention, the dyeing time is extremely shortened compared to the conventional exhaust dyeing method that does not use the above-mentioned special dedicated equipment, and therefore energy consumption such as power consumption and steam consumption is reduced, resulting in a reduction in CO 2 In addition, the dyeing method of the present invention is economically effective because it simplifies the dyeing operation without requiring investment in related equipment, as compared with the conventional exhaust dyeing method using special dedicated equipment, and can give uniform dyed products with high fastness that are comparable to those of the conventional exhaust dyeing method. 2 This is a new method for dyeing cellulosic fiber fabrics that simplifies dyeing operations while reducing emissions and can produce uniformly dyed products with high color fastness and no color unevenness. [Brief description of the drawings]

[0014] [Figure 1] FIG. 1 is a schematic diagram of a jet dyeing machine that can be used in the dyeing method of the present invention. [Diagram 2] 1 is a table showing the timing of introduction and elapsed time in Examples 1 to 4, and a graph showing the relationship between time and temperature. [Diagram 3] 11 is a table showing the timing of introduction and elapsed time in Example 5, and a graph showing the relationship between time and temperature. [Figure 4] 1 is a table showing the timing of introduction and elapsed time in Example 6, and a graph showing the relationship between time and temperature. [Diagram 5] 13 is a table showing the timing of introduction and elapsed time in Example 7, and a graph showing the relationship between time and temperature. [Figure 6] 1 is a table showing the timing of introduction and elapsed time in Examples 8 and 9, and a graph showing the relationship between time and temperature. [Figure 7] 1 is a table showing the timing of introduction and elapsed time in Examples 10 to 12, and a graph showing the relationship between time and temperature. [Figure 8] 1 is a table showing the timing of introduction and elapsed time in Example 13, and a graph showing the relationship between time and temperature. [Figure 9] 1 is a table showing the timing of introduction and elapsed time in Example 14, and a graph showing the relationship between time and temperature. [Figure 10] 1 is a table showing the timing of introduction and elapsed time in Example 15, and a graph showing the relationship between time and temperature. [Figure 11] 1 is a table showing the timing of introduction and elapsed time in Comparative Example 1, and a graph showing the relationship between time and temperature. [Figure 12] 1 is a table showing the timing of introduction and elapsed time in Comparative Example 2, and a graph showing the relationship between time and temperature. [Figure 13] 13 is a table showing the timing of introduction and elapsed time in Comparative Example 3, and a graph showing the relationship between time and temperature. [Figure 14] 13 is a table showing the timing of introduction and elapsed time in Comparative Example 4, and a graph showing the relationship between time and temperature. [Figure 15] 13 is a table showing the timing of introduction and elapsed time in Comparative Example 5, and a graph showing the relationship between time and temperature. [Figure 16] 1 is a table showing the timing of introduction and elapsed time in Comparative Example 6, and a graph showing the relationship between time and temperature. [Figure 17]13 is a table showing the timing of introduction and elapsed time in Comparative Example 7, and a graph showing the relationship between time and temperature. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0015] Hereinafter, an embodiment of the present invention will be described in detail. One embodiment of the present invention is a method for dyeing cellulosic fibers or textile products comprising cellulosic fibers, comprising the steps of: supplying water in a first temperature range of 5° C. or more and less than 30° C., or in a second temperature range of 30° C. or more and less than 40° C., and simultaneously introducing a textile product of or containing cellulosic fibers into the dyebath, regardless of whether the introduction of water occurs before or after the introduction of water; a temperature increasing step of increasing the temperature from the first temperature region to a second temperature region of 30° C. or more and less than 40° C., and from the second temperature region to a third temperature region of 40° C. or more and 70° C. or less, or from the second temperature region to a third temperature region of 40° C. or more and 70° C. or less; maintaining the third temperature within the third temperature range for a predetermined period of time; dosing a reactive dye at a temperature equal to or greater than the first temperature range; and a step of adding a mixture of an inorganic salt and an alkali agent in three or more portions at a temperature equal to or higher than the second temperature region, separately from the step of adding the reactive dye; The number of divided doses is preferably 5 or less.

[0016] The form of the cellulose-based fiber or the textile product containing the cellulose-based fiber to be dyed by the dyeing method of the present embodiment is not particularly limited, and various forms such as thread, woven fabric, weft knitted fabric, nonwoven fabric, sewn product, etc. are exemplified. The cellulose-based fiber is also not particularly limited, and examples thereof include cotton, hemp, rayon, cuprammonium rayon, lyocell, organic solvent cellulose fiber, and ionic liquid cellulose fiber, but preferably cotton, rayon, cuprammonium rayon, lyocell, and organic solvent cellulose fiber, and more preferably cotton and rayon. Fibers other than the cellulose-based fiber of the textile product containing the cellulose-based fiber to be dyed by the dyeing method of the present embodiment can be dyed in combination with a known dyeing method.

[0017] The equipment used in the dyeing method of the present embodiment is not particularly limited, but is preferably a cheese dyeing machine, a skein dyeing machine, a liquid flow dyeing machine, a gas flow dyeing machine, a beam dyeing machine, a jigger dyeing machine, a winch dyeing machine, a rotary dyeing machine, or a paddle dyeing machine, more preferably a cheese dyeing machine, a skein dyeing machine, a liquid flow dyeing machine, a beam dyeing machine, a jigger dyeing machine, or a winch dyeing machine, even more preferably a cheese dyeing machine, a skein dyeing machine, a liquid flow dyeing machine, or a winch dyeing machine, and most preferably a liquid flow dyeing machine. FIG. 1 shows an outline of a liquid flow dyeing machine. The dyeing equipment is preferably equipped with a temperature raising and temperature adjusting device, an agitating device, and a reserve tank 2 that has a function of preparing and storing a mixture (solution) of inorganic salts and alkaline agents in advance and adding the mixture (solution) to the dye bath of the dyeing equipment in portions, and that stores a solution in which both inorganic salts and alkaline agents are dissolved. By using the liquid flow dyeing machine 1 illustrated in FIG. 1, the dyeing reaction can be efficiently carried out by feeding (adding) the solution in which both inorganic salts and alkaline agents are dissolved in the reserve tank 2 to the dyeing solution through the nozzle 4 while moving the fabric 5 while adjusting the temperature of the dye bath 6 with the heat exchanger 3. In addition, a solution in which reactive dyes are dissolved is prepared in the reserve tank and fed into the dyeing device, and then a solution in which a mixture (solution) of inorganic salts and alkaline agents is dissolved is prepared and fed into the dyeing device, and then a solution in which a mixture (solution) of inorganic salts and alkaline agents is dissolved is prepared and fed into the dyeing device, making it possible to feed the mixture of inorganic salts and alkaline agents in three or more separate portions in addition to the step of feeding the reactive dyes. The number of separate portions is preferably five or less.

[0018] The dyeing method of the present embodiment includes a step of supplying water in a first temperature range of 5° C. or more and less than 30° C., or a second temperature range of 30° C. or more and less than 40° C., to a dyebath, and adding a textile product of or containing cellulosic fibers. Here, the water supply and the addition can be performed before or after the water supply. The first temperature range is preferably 5°C or higher and lower than 30°C, which is the environmental temperature. If the temperature is lower than 5°C, the energy consumption required for heating becomes large, so the CO 2 emissions will increase.

[0019] The dyeing method of the present embodiment includes a temperature increasing step of increasing the temperature from a first temperature region to a second temperature region of 30°C or more and less than 40°C, and from the second temperature region to a third temperature region of 40°C or more and 70°C or less, or from the second temperature region to the third temperature region of 40°C or more and 70°C or less. The second temperature range is preferably 30° C. or higher and lower than 40° C. If the temperature is lower than 30° C., the reaction rate of the reactive dye decreases, so that it may be difficult to obtain the desired hue concentration or the fastness may decrease. If the temperature is higher than 40° C., the energy consumption required for heating increases, and as a result, CO 2 emissions will increase. The third temperature range is preferably 40° C. or higher and 70° C. or lower, and more preferably 40° C. or higher and 60° C. or lower. If the temperature is lower than 40° C., the reaction rate of the reactive dye decreases, so that it may be difficult to obtain the desired hue concentration or the fastness may decrease. If the temperature exceeds 70° C., the energy consumption required for heating increases, and as a result, CO 2 emissions will increase.

[0020] The dyeing method of the present embodiment includes a step of maintaining the third temperature in the third temperature region for a predetermined period of time. The time for the third temperature holding step in which the dye is held in the third temperature range is preferably 10 minutes or more and 70 minutes or less. If the time is less than 10 minutes, the reaction rate of the reactive dye decreases, so that it may be difficult to obtain the desired hue concentration or the fastness may decrease. If the time is more than 70 minutes, the energy consumption such as the electricity required to operate the equipment and the amount of steam required to maintain the temperature of the dye bath increases, and as a result, the CO 2 emissions will increase. The dyeing method of the present embodiment may further include a step of maintaining the temperature in the second temperature range for a predetermined period of time. The time of the second temperature maintaining step of maintaining the temperature in the second temperature range is preferably 10 minutes or more and 70 minutes or less.

[0021] The heating rate in the heating process from the first temperature region to the second temperature region and from the second temperature region to the third temperature region is not particularly limited, but is preferably 1°C / min or more and 4°C / min or less, and more preferably 1°C / min or more and 2°C / min or less. The dyeing method of the present embodiment includes a step of adding a reactive dye at a temperature equal to or higher than the first temperature range, provided that the addition of a mixture of an inorganic salt and an alkali agent is started after the start of the addition of the reactive dye.

[0022] The dyeing method of the present embodiment includes a step of dividing and adding a mixture of inorganic salts and an alkaline agent in three or more portions at a temperature equal to or higher than the second temperature range, in addition to the step of adding a reactive dye. The number of divided doses is preferably five or less. If inorganic salts and alkaline agents are added without being mixed, each addition takes time, and energy consumption such as the electricity required to operate the equipment and the amount of steam required to maintain the temperature of the dye bath increases, which leads to an increase in CO 2 If the reactive dye is added in one go without being divided, it will be instantly absorbed by the cellulosic fibers, resulting in significant color unevenness in the dyed product, and therefore it will be impossible to evaluate the color fastness. In addition, if the number of divided doses is six or more, it will take a long time, so the energy consumption, such as the electricity required to operate the equipment and the amount of steam required to maintain the temperature of the dye bath, will increase, and the CO 2 emissions will increase. It is preferable that all of the mixture of the inorganic salt and the alkaline agent is added in portions within the third temperature region, or that all of the mixture of the inorganic salt and the alkaline agent is added in portions within the second temperature region. The divided addition may be performed during the temperature-raising step, but in that case, since the temperature-raising operation and the addition operation must be performed in parallel, from the viewpoint of suppressing color unevenness, it is preferable to complete all divided additions within the second temperature region or the third temperature region where the temperature is maintained within a predetermined range. The time interval for the divided addition is preferably 5 to 17 minutes, more preferably 7 to 15 minutes, and even more preferably 8 to 12 minutes, from the viewpoint of controlling the dyeing reaction and from the viewpoint of workability. The dyeing reaction time period from the final stage of divided addition to the end of the third temperature holding step is preferably 20 to 50 minutes, more preferably 40 to 50 minutes. If it is less than 20 minutes, the reaction rate of the reactive dye decreases, so that it may be difficult to obtain the desired hue concentration or the fastness may decrease. If it exceeds 50 minutes, the energy consumption such as the electricity required to operate the equipment and the amount of steam required to hold the temperature of the dye bath increases, and as a result, the CO 2 emissions will increase.

[0023] There is no particular restriction on the ratio of divisions, but the divisions are added three or more times and five or less times. When the total amount of the mixture of inorganic salts and alkaline agent is T (g), the amount added in the first stage is A (g), and the amount added in the second stage is B (g), the following formulas (1) to (3): 1 / 20×T≦A≦5 / 20×T…Formula (1) 1 / 20×T≦B≦7 / 20×T…Formula (2) A≦B…Formula (3) It is preferable that the following is satisfied. If the formulae (1) to (3) are not satisfied, color unevenness may occur, making it impossible to obtain a uniformly dyed product, and fastness may decrease.

[0024] In the dyeing method of the present embodiment, the total time period from the water supply to the end of the third temperature holding step is preferably 100 minutes or less, and more preferably 80 minutes or less. In the dyeing method of the present embodiment, the rotation speed of the knitted fabric is preferably set to 30 seconds / cycle to 180 seconds / cycle from the viewpoint of suppressing uneven dyeing and suppressing deterioration of surface quality.

[0025] The dyeing solution (dyeing solution) in the dye bath used in the dyeing method of this embodiment can contain one or more reactive dyes and, if desired, components such as dispersants, wetting agents, bath softeners, bath smoothing agents, and emulsifiers. Examples of reactive dyes include reactive dyes having at least one functional group that reacts with cellulosic fibers, such as monochlorotriazinyl, monofluorotriazinyl, fluorochloropyrimidinyl, dichloroquinoxanyl, vinylsulfonyl, and sulfatoethylsulfonyl functional groups, or polyfunctional dyes having a plurality of such functional groups, which react with cellulosic fibers at a temperature of 20° C. to 100° C. and a pH of 8 to 13. In addition, the dye addition step in which the reactive dye is added is preferably carried out before the divided addition of the mixture of inorganic salts and alkaline agents.

[0026] Examples of inorganic salts used in the dyeing method of the present embodiment include, but are not limited to, sodium sulfate, potassium sulfate, sodium chloride, potassium chloride, mixtures thereof, etc. Examples of alkaline agents include, but are not limited to, sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide, sodium metasilicate, trisodium phosphate, tripotassium phosphate, mixtures thereof, etc. The amounts of inorganic salts and alkaline agents added are determined by the weight of the item to be dyed, the hue concentration, and the liquor ratio (weight of the item to be dyed: weight of the dyeing solution (calculated assuming specific gravity of 1)). The total amount of inorganic salts added (g / L (dyeing solution)) is usually 1 to 200 g / L, preferably 1 to 100 g / L, and more preferably 1 to 80 g / L. The total amount of alkaline agents added (g / L) is usually 0.1 to 50 g / L, and preferably 1 to 20 g / L. The liquor ratio is usually 1:1 to 1:100, preferably 1:5 to 1:30.

[0027] The dyeing method of this embodiment is completed when the third temperature holding step is completed, and then the dyeing solution is discharged from the dyebath, followed by a washing step to remove the remaining dye. The washing step may be a known method, and may be any combination of at least one water washing step at a bath ratio of 1:5 or more and a temperature of 10°C to 40°C for 5 minutes or more, and at least one hot water washing step at a bath ratio of 1:5 or more and a temperature of 60°C or more for 5 minutes or more. EXAMPLES

[0028] The present invention will be specifically described below with reference to examples and comparative examples, but the present invention is not limited to these examples. 2 The calculation of the emission reduction amount and various evaluations of each yarn or textile product were carried out using the following methods.

[0029] (1)CO 2 Calculating Emissions Reductions The power consumption and steam consumption required for the operation of the dyeing machine were measured and calculated using the following formula: W=E×α+S×β {where, W:CO 2 Emissions (kg-CO 2 e), E: power consumption (MJ), S: steam consumption (MJ), α: CO2 of electricity 2 Basic unit (kg-CO 2 e / MJ), and β: steam CO 2 Basic unit (kg-CO 2 e / MJ). 2 Emissions (kg-CO 2 e) was calculated, where α and β are the CO 2 This is the basic unit (kg-CO2e / MJ) and is the value published by the Ministry of the Environment. 2 The basic unit is not particularly limited, but may be the CO2 in the above-mentioned Non-Patent Document 1: "Reference Material 2: List of formulas and emission coefficients for calculating greenhouse gas emissions (https: / / www.env.go.jp / earth / ondanka / suishin_g / 3rd_edition / ref2.pdf)" 2For example, the basic unit of electricity, α, is 0.1542 (kg-CO 2 e / MJ), and the steam consumption unit β is 0.0600 (kg-CO 2 In the following examples and comparative examples, α=0.1542 (kg-CO 2 e / MJ), β=0.0600(kg-CO 2 e / MJ) to reduce CO 2 Emissions (kg-CO 2 e) was calculated. 2 Emissions are 30 (kg-CO 2 e) If less than CO 2 Emissions have been reduced by 30(kg-CO 2 e) If it is more than CO 2 It was determined that emissions had not been reduced.

[0030] (2) Uneven color (spots) Five randomly selected points from the dyed textile product were measured using a spectrophotometer (Gretagmacbeth, Color-Eye7000A) under conditions of D56 light source and a viewing angle of 10 degrees, and the L*, a*, and b* values ​​in the CIE1976L*a*b* color space were calculated. Next, for all 10 combinations in which two points were selected from the five measured points, the ΔL*, Δa*, and Δb* values, which are the differences between the L*, a*, and b* values ​​of the two selected points, were calculated and expressed by the following formula: ΔE=((ΔL*)^2+(Δa*)^2+(Δb*)^2)^1 / 2 The ΔE value for each was calculated by the method described above, and the maximum ΔE value was calculated from the 10 ΔE values. If this maximum ΔE value was 1.5 or more, it was determined that there was color unevenness, and if it was less than 1.5, it was determined that there was no color unevenness.

[0031] (3) Dye fastness to sweat A sweat fastness test was conducted in accordance with the sweat color fastness test method specified in JIS L 0848, with grades 4 and above being "good," grades below 4 being "poor," and dyed textile products with uneven coloring (spots) being "unrecognizable." In addition, a multi-fiber woven fabric made by interweaving eight types of fibers (cotton, nylon, acetate, wool, rayon, acrylic, silk, and polyester) in a vertical stripe pattern conforming to JIS L 0803 was used as the attached white cloth.

[0032] [Example 1] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, the liquid temperature was then adjusted to 40°C, which is the third temperature range, and 0.26 parts of reactive dye Procion Red H-E3B manufactured by DyStar, which had been dissolved in advance, was fed as the dye-feeding step. Next, as the first-stage divided-feeding step, a solution in which 2 / 20 of 5 parts of anhydrous Glauber's salt and 2 / 20 of 1.5 parts of sodium carbonate, which had been dissolved in advance, were mixed and fed within 10 minutes. 10 minutes after the start of the first-stage feeding, a solution in which 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate, which had been dissolved in advance, were mixed and fed within 10 minutes as the second-stage divided-feeding step. Ten minutes after the start of the second stage addition, a solution of 5 parts of anhydrous Glauber's salt in an amount of 12 / 20 and 1.5 parts of sodium carbonate in an amount of 12 / 20 that had been dissolved in advance was added within 10 minutes as a third stage divided addition step. Ten minutes after the start of the third stage addition, the liquid temperature was heated to 60°C, which is the third temperature range, in 10 minutes, and dyeing was performed at 60°C for 30 minutes, after which the dyeing liquid was discharged, and then washing was performed by a known method and drying was performed to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 2, and the evaluation results are shown in Table 1 below.

[0033] [Example 2] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dye added in the first stage in the divided addition step were 1 / 20 of 5 parts of anhydrous Glauber's salt and 1 / 20 of 1.5 parts of sodium carbonate, the amounts of the dye added in the second stage were 3 / 20 of 5 parts of anhydrous Glauber's salt and 3 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dye added in the third stage were 16 / 20 of 5 parts of anhydrous Glauber's salt and 16 / 20 of 1.5 parts of sodium carbonate. Then, the dyeing solution was discharged, and the dyed product was washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 2, and the evaluation results are shown in Table 1 below.

[0034] [Example 3] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dye added in the first stage in the divided addition step were 1 / 20 of 5 parts of anhydrous Glauber's salt and 1 / 20 of 1.5 parts of sodium carbonate, the amounts of the dye added in the second stage were 7 / 20 of 5 parts of anhydrous Glauber's salt and 7 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dye added in the third stage were 12 / 20 of 5 parts of anhydrous Glauber's salt and 12 / 20 of 1.5 parts of sodium carbonate. Then, the dyeing solution was discharged, and the dyed product was washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 2, and the evaluation results are shown in Table 1 below.

[0035] [Example 4] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dye added in the first stage in the divided addition step were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate, the amounts of the dye added in the second stage were 7 / 20 of 5 parts of anhydrous Glauber's salt and 7 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dye added in the third stage were 8 / 20 of 5 parts of anhydrous Glauber's salt and 8 / 20 of 1.5 parts of sodium carbonate. Then, the dyeing solution was discharged, and the dyed product was washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2The table e) and a graph showing the relationship between time and temperature are shown in FIG. 2, and the evaluation results are shown in Table 1 below.

[0036] [Example 5] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, and the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, after which 0.26 parts of pre-dissolved reactive dye Procion Red H-E3B manufactured by DyStar was fed, and the liquid temperature was heated to 60°C, which is the third temperature range, in 20 minutes. Next, as the first stage divided feeding step, a solution in which 2 / 20 of 5 parts of anhydrous Glauber's salt and 2 / 20 of 1.5 parts of sodium carbonate were mixed and fed within 10 minutes. 10 minutes after the start of the first stage feeding, a solution in which 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate were mixed and fed within 10 minutes as the second stage divided feeding step. Ten minutes after the start of the second stage, a solution of 12 / 20 of 5 parts of anhydrous Glauber's salt and 1.5 parts of sodium carbonate was added within 10 minutes as a third stage divided addition step. After dyeing for 20 minutes at 60°C from the start of the third stage addition, the dyeing solution was discharged, and then washing was performed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 3, and the evaluation results are shown in Table 1 below.

[0037] [Example 6] The dyeing was carried out in the same manner as in Example 5, except that the dyeing was carried out at 60° C. for 30 minutes from the start of the third stage in the divided addition process, and the dyeing solution was then discharged, and the dyed product was then washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 4, and the evaluation results are shown in Table 1 below.

[0038] [Example 7] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, and the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, after which 0.26 parts of pre-dissolved reactive dye Procion Red H-E3B manufactured by DyStar was fed, and the liquid temperature was heated to 50°C, which is the third temperature range, in 10 minutes. Next, as the first stage divided feeding step, a solution in which 2 / 20 of 5 parts of anhydrous Glauber's salt and 2 / 20 of 1.5 parts of sodium carbonate were mixed and fed within 10 minutes. 10 minutes after the start of the first stage feeding, a solution in which 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate were mixed and fed within 10 minutes as the second stage divided feeding step. Ten minutes after the start of the second stage, a solution of 12 / 20 of 5 parts of anhydrous Glauber's salt and 1.5 parts of sodium carbonate was added within 10 minutes as a third stage divided addition step. After dyeing for 50 minutes at 50°C from the start of the third stage addition, the dyeing solution was discharged, and then washing was performed by a known method and drying was performed to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 5, and the evaluation results are shown in Table 1 below.

[0039] [Example 8] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dyeing liquid were discharged after dyeing, and then the dyeing operation was carried out by a known method and the dyed product was dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 6, and the evaluation results are shown in Table 1 below.

[0040] [Example 9] The dyeing was carried out in the same manner as in Example 8, except that the amounts of the dye added in the first stage in the divided addition step were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate, the amounts of the dye added in the second stage were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate, the amounts of the dye added in the third stage were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dye added in the fourth stage were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate. The dyeing was then carried out, and the dyeing solution was discharged, and the dyed product was then washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 6, and the evaluation results are shown in Table 2 below.

[0041] [Example 10] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dyed material added in the first stage in the divided addition step were 2 / 20 of 5 parts of anhydrous Glauber's salt and 2 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the second stage were 3 / 20 of 5 parts of anhydrous Glauber's salt and 3 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the third stage were 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the fourth stage were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dyed material added in the fifth stage were 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate. The dyeing was then carried out, and the dyeing solution was discharged, and the material was washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 Table e) and a graph showing the relationship between time and temperature are shown in FIG. 7, and the evaluation results are shown in Table 2 below.

[0042] [Example 11] The dyeing was carried out in the same manner as in Example 10, except that the amounts of the dyed material added in the first stage in the divided addition step were 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the second stage were 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the third stage were 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the fourth stage were 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dyed material added in the fifth stage were 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate. The dyeing was then carried out, and the dyeing solution was discharged, followed by washing and drying by a known method to obtain a dyed product. 2 Emissions (kg-CO 2 Table e) and a graph showing the relationship between time and temperature are shown in FIG. 7, and the evaluation results are shown in Table 2 below.

[0043] [Example 12] The dyeing was carried out in the same manner as in Example 10, except that the amounts of the dyed material added in the first stage in the divided addition step were 1 / 20 of 5 parts of anhydrous Glauber's salt and 1 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the second stage were 1 / 20 of 5 parts of anhydrous Glauber's salt and 1 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the third stage were 3 / 20 of 5 parts of anhydrous Glauber's salt and 3 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the fourth stage were 3 / 20 of 5 parts of anhydrous Glauber's salt and 3 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dyed material added in the fifth stage were 12 / 20 of 5 parts of anhydrous Glauber's salt and 12 / 20 of 1.5 parts of sodium carbonate. The dyeing was then carried out, and the dyeing solution was discharged, followed by washing and drying by a known method to obtain a dyed product. 2 Emissions (kg-CO 2 Table e) and a graph showing the relationship between time and temperature are shown in FIG. 7, and the evaluation results are shown in Table 2 below.

[0044] [Example 13] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, the liquid temperature was then adjusted to 40°C, which is the third temperature range, and 0.26 parts of reactive dye Procion Red H-E3B manufactured by DyStar, which had been dissolved in advance, was fed as the dye-feeding step. Next, as the first-stage divided-feeding step, a solution in which 2 / 20 of 5 parts of anhydrous Glauber's salt and 2 / 20 of 1.5 parts of sodium carbonate, which had been dissolved in advance, were mixed and fed within 17 minutes. 17 minutes after the start of the first-stage feeding, a solution in which 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate, which had been dissolved in advance, were mixed and fed within 17 minutes as the second-stage divided-feeding step. 17 minutes after the start of the second stage addition, a solution of 12 / 20 of 5 parts of anhydrous Glauber's salt and 1.5 parts of sodium carbonate, which had been dissolved in advance, was mixed and added within 17 minutes as the third stage divided addition step. 17 minutes after the start of the third stage addition, the liquid temperature was heated to 60°C, which is the third temperature range, in 10 minutes, and dyeing was performed at 60°C for 30 minutes, after which the dyeing liquid was discharged, and then washing was performed by a known method and drying was performed to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 8, and the evaluation results are shown in Table 2 below.

[0045] [Example 14] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, the liquid temperature was then adjusted to 40°C, which is the third temperature range, and 0.26 parts of DyStar's reactive dye Procion Red H-E3B, ​​which had been dissolved in advance, was fed as the dye-feeding step. Next, as the first-stage divided-feeding step, a solution in which 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, which had been dissolved in advance, were mixed and fed within 5 minutes. Five minutes after the start of the first-stage feeding, as the second-stage divided-feeding step, a solution in which 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate, which had been dissolved in advance, were mixed and fed within 5 minutes. Five minutes after the start of the second stage, a solution containing 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate dissolved in advance was added within 5 minutes as a third stage divided addition step. Five minutes after the start of the third stage, a solution containing 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate dissolved in advance was added within 5 minutes as a fourth stage divided addition step. Five minutes after the start of the fourth stage, a solution containing 4 / 20 of 5 parts of anhydrous Glauber's salt and 4 / 20 of 1.5 parts of sodium carbonate dissolved in advance was added within 5 minutes as a fifth stage divided addition step. Five minutes after the start of the fifth stage, the liquid temperature was heated to 60°C, which is the third temperature range, in 10 minutes, and dyed at 60°C for 30 minutes, after which the dyeing liquid was discharged, and then washed by a known method and dried to obtain a dyed product. Addition timing, elapsed time, CO 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 9, and the evaluation results are shown in Table 2 below.

[0046] [Example 15] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dyed material added in the first stage in the divided addition step were 1 / 20 of 5 parts of anhydrous Glauber's salt and 1 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the second stage were 1 / 20 of 5 parts of anhydrous Glauber's salt and 1 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the third stage were 3 / 20 of 5 parts of anhydrous Glauber's salt and 3 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the fourth stage were 3 / 20 of 5 parts of anhydrous Glauber's salt and 3 / 20 of 1.5 parts of sodium carbonate, the amounts of the dyed material added in the fifth stage were 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dyed material added in the sixth stage were 6 / 20 of 5 parts of anhydrous Glauber's salt and 6 / 20 of 1.5 parts of sodium carbonate. After dyeing, the dyeing solution was discharged, and then washing was carried out by a known method and the material was dried to obtain a dyed product. Figure 10 shows a table of the input timing, elapsed time, and CO2 emissions (kg-CO2e), as well as a graph showing the relationship between time and temperature, and the evaluation results are shown in Table 2 below.

[0047] [Comparative Example 1] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, the liquid temperature was then adjusted to 40°C, which is the third temperature range, and 0.26 parts of reactive dye Procion Red H-E3B manufactured by DyStar, which had been dissolved in advance, was fed as the dye-feeding step. Next, as the first-stage salt-feeding step, 2 / 20 of the amount of 5 parts of anhydrous Glauber's salt that had been dissolved in advance was fed within 5 minutes. Five minutes after the start of the first-stage salt-feeding, 6 / 20 of the amount of 5 parts of anhydrous Glauber's salt that had been dissolved in advance was fed within 5 minutes as the second-stage salt-feeding step. Five minutes after the start of the second-stage salt-feeding, 12 / 20 of the amount of 5 parts of anhydrous Glauber's salt that had been dissolved in advance was fed within 5 minutes as the third-stage salt-feeding step. Next, 5 minutes after the start of the third stage salt addition, 2 / 20 of the amount of 5 parts of sodium carbonate dissolved in advance was added within 5 minutes as the first stage alkaline agent addition step. 5 minutes after the start of the first stage addition, 6 / 20 of the amount of 5 parts of sodium carbonate dissolved in advance was added within 5 minutes as the second stage alkaline agent addition step. 5 minutes after the start of the second stage addition, 12 / 20 of the amount of 5 parts of sodium carbonate dissolved in advance was added within 5 minutes as the third stage alkaline agent addition step. 5 minutes after the start of the third stage alkaline agent addition, the liquid temperature was heated to 60°C, which is the third temperature range, in 10 minutes, and dyed at 60°C for 30 minutes, after which the dyeing liquid was discharged, and then washed by a known method and dried to obtain a dyed product. Addition timing, elapsed time, CO 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 11, and the evaluation results are shown in Table 3 below.

[0048] [Comparative Example 2] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, and the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle. After the liquid temperature was raised to 40°C, which is the third temperature range, 0.26 parts of reactive dye Procion Red H-E3B, ​​manufactured by DyStar, which had been dissolved in advance, was then fed in as a dye-feeding step. Next, a solution of 5 parts of anhydrous Glauber's salt and 1.5 parts of sodium carbonate, which had been dissolved in advance, was fed in one go without dividing. 30 minutes after the feeding of the mixed solution of anhydrous Glauber's salt and sodium carbonate, the liquid temperature was heated to 60°C, which is the third temperature range, in 10 minutes, and dyed at 60°C for 30 minutes, after which the dyeing liquid was discharged, and then washed by a known method and dried to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 12, and the evaluation results are shown in Table 3 below.

[0049] [Comparative Example 3] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, and the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle. Then, 0.26 parts of a pre-dissolved reactive dye Procion Red H-E3B manufactured by DyStar was fed, and the liquid temperature was heated to 60°C, which is the third temperature range, in 20 minutes. Next, as the first stage of salt division feeding step, 2 / 20 of the amount of 5 parts of anhydrous Glauber's salt that had been pre-dissolved was fed within 10 minutes. 10 minutes after the start of the first stage of salt feeding, 6 / 20 of the amount of 5 parts of anhydrous Glauber's salt that had been pre-dissolved was fed within 10 minutes as the second stage of salt feeding step. 10 minutes after the start of the second stage of salt feeding, 12 / 20 of the amount of 5 parts of anhydrous Glauber's salt that had been pre-dissolved was fed within 10 minutes as the third stage of salt feeding step. Next, 30 minutes after the start of the third stage salt addition, 2 / 20 of the amount of 5 parts of sodium carbonate dissolved in advance was added within 10 minutes as the first stage alkaline agent addition step. 10 minutes after the start of the first stage addition, 6 / 20 of the amount of 5 parts of sodium carbonate dissolved in advance was added within 10 minutes as the second stage alkaline agent addition step. 10 minutes after the start of the second stage addition, 12 / 20 of the amount of 5 parts of sodium carbonate dissolved in advance was added as the third stage alkaline agent addition step. After dyeing for 70 minutes at 60°C from the start of the third stage alkaline agent addition, the dyeing solution was discharged, and then washing was performed by a known method and dried to obtain a dyed product. Addition timing, elapsed time, CO 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 13, and the evaluation results are shown in Table 3 below.

[0050] [Comparative Example 4] 100 parts of water at 20°C, which is the first temperature range, was fed into the jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, and the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle. After the liquid temperature was raised to 40°C, which is the third temperature range, 0.26 parts of reactive dye Procion Red H-E3B, ​​manufactured by DyStar, which had been dissolved in advance, was then fed in as a dye-feeding step. Next, a solution of 5 parts of anhydrous Glauber's salt and 1.5 parts of sodium carbonate, which had been dissolved in advance, was fed in its entirety in one go without being divided. Immediately after the feeding of the mixed solution of anhydrous Glauber's salt and sodium carbonate, the liquid temperature was heated to 60°C, which is the third temperature range, in 20 minutes, and dyed at 60°C for 30 minutes, after which the dyeing liquid was discharged, and then washed by a known method and dried to obtain a dyed product. The feeding timing, elapsed time, CO 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 14, and the evaluation results are shown in Table 3 below.

[0051] [Comparative Example 5] 100 parts of water at 20°C, which is the first temperature range, was fed into the liquid jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle, the liquid temperature was then adjusted to 40°C, which is the third temperature range, and 0.26 parts of DyStar's reactive dye Procion Red H-E3B, ​​which had been dissolved in advance, was fed as a dye-feeding step. Next, 5 parts of anhydrous sodium sulfate and 1.5 parts of sodium carbonate, which had been dissolved in advance, were fed over 30 minutes at a linear speed of 1 / 30 parts per minute using a dedicated device for adding chemicals to a dye bath that can be metered in real time. After the feeding was completed, the liquid temperature was set to 40°C for 90 minutes, and the dyeing liquid was discharged, followed by washing and drying by a known method to obtain a dyed product. The feeding timing, elapsed time, and CO 2 Emissions (kg-CO 2 The table of e) and a graph showing the relationship between time and temperature are shown in FIG. 15, and the evaluation results are shown in Table 3 below.

[0052] [Comparative Example 6] 100 parts of water at 20°C, which is the first temperature range, was fed into the liquid jet dyeing machine, 5 parts of knitted fabric made of unmercerized cotton was fed, and the rotation speed of the knitted fabric was adjusted to 90 seconds / cycle. Then, 0.26 parts of DyStar's reactive dye Procion Red H-E3B, ​​which had been dissolved in advance, was fed, and the liquid temperature was heated to 60°C, which is the third temperature range, in 2.5 minutes. Next, 5 parts of anhydrous sodium sulfate and 1.5 parts of sodium carbonate, which had been dissolved in advance, were fed over 15 minutes at a linear speed of 1 / 15 parts per minute using a dedicated device for adding chemicals to a dye bath that can be metered in real time. After the feeding was completed, the liquid was dyed at 60°C for 20 minutes, and then the dyeing liquid was discharged, and then the washing operation was performed by a known method, and the dyed product was obtained by drying. The timing of feeding, elapsed time, CO 2 Emissions (kg-CO 2 The table of e) and a graph showing the relationship between time and temperature are shown in FIG. 16, and the evaluation results are shown in Table 3 below.

[0053] [Comparative Example 7] The dyeing was carried out in the same manner as in Example 1, except that the amounts of the dye added in the first stage in the divided addition step were 5 / 20 of 5 parts of anhydrous Glauber's salt and 5 / 20 of 1.5 parts of sodium carbonate, and the amounts of the dye added in the second stage were 15 / 20 of 5 parts of anhydrous Glauber's salt and 15 / 20 of 1.5 parts of sodium carbonate. After dyeing, the dyeing solution was discharged, and then washing was carried out by a known method and drying was carried out to obtain a dyed product. 2 Emissions (kg-CO 2 The table e) and a graph showing the relationship between time and temperature are shown in FIG. 17, and the evaluation results are shown in Table 3 below.

[0054] The dyed products obtained in Examples 1 to 15 and Comparative Examples 1 to 7 were subjected to CO 2 The amount of emission reduction was calculated, and evaluations of color unevenness and color fastness were carried out. The evaluation results are shown in Tables 1 to 3 below.

[0055] [Table 1]

[0056] [Table 2]

[0057] [Table 3]

[0058] In Examples 1 to 15, CO 2 It can be seen that the amount of discharged dye is significantly reduced, the dyed products obtained are uniformly dyed without unevenness in color, and furthermore have high color fastness. In the dyeing method of Comparative Example 1, in which the time was reduced and salt and alkali were added separately instead of mixed together, and in the dyeing methods of Comparative Examples 2 and 4, in which the time was reduced and salt and alkali were added all at once instead of separately, 2 While emissions were significantly reduced, the resulting dyed products had significant color unevenness, making it impossible to evaluate the color fastness. In the dyeing method of Comparative Example 3, the dyed product obtained was dyed uniformly without color unevenness and had high fastness, but it took a long time to dye the product, and the dyeing process was difficult to perform. 2 Emissions have increased. In the dyeing method of Comparative Example 5, the dyed product obtained was dyed uniformly without unevenness in color and had high fastness, but it took a long time to dye the product, and the dyeing process was difficult to perform. 2 The amount of discharged material increased. In addition, the number of times that the mixing and dividing step is divided is 30 times, which is very large, so it is impossible to do it by hand, and it is not versatile because it requires dedicated equipment to add chemicals to the dye bath that can be measured in real time at a linear speed of 1 / 30 parts per minute. In the dyeing method of Comparative Example 6, CO 2 While the amount of emissions was significantly reduced, the dyed products obtained had strong color unevenness, and the color fastness could not be evaluated.In addition, the number of times that the mixing and dividing step was divided was 30, which was very large, making it impossible to do by hand, and it required dedicated equipment to add chemicals to the dye bath that could be metered in real time at a linear speed of 1 / 30 parts per minute, making it less versatile. In the dyeing method of Comparative Example 7, in which the number of times of mixing and dividing was limited to two to shorten the time, 2While emissions were significantly reduced, the resulting dyed products had significant color unevenness, making it impossible to evaluate the color fastness. [Industrial Applicability]

[0059] The present invention shortens the staining time, and 2 The present invention can provide a novel dyeing method that can reduce emissions of dyes, effectively simplify dyeing operations, and give uniform dyed products with high fastness. Therefore, the present invention can be suitably used in dyeing textile products containing cellulose-based fibers. [Explanation of symbols]

[0060] 1 Jet dyeing machine 2 Reserve tank 3 Heat exchanger 4 Nozzles 5. Fabric 6 Dyeing bath

Claims

1. A method for dyeing cellulosic fibers or textile products containing cellulosic fibers, comprising the steps of: A step of supplying water in a first temperature range of 5° C. or more and less than 30° C., or a second temperature range of 30° C. or more and less than 40° C., and simultaneously introducing a fiber product of or containing a cellulosic fiber into a dyebath, wherein the water introduction and the introduction can be performed before or after the water introduction; a temperature increasing step of increasing the temperature from the first temperature region to a second temperature region of 30° C. or more and less than 40° C., and from the second temperature region to a third temperature region of 40° C. or more and 70° C. or less, or from the second temperature region to a third temperature region of 40° C. or more and 70° C. or less; maintaining the third temperature within the third temperature range for a predetermined period of time; dosing a reactive dye at a temperature equal to or greater than the first temperature range; and a step of adding a mixture of an inorganic salt and an alkali agent in three or more portions at a temperature equal to or higher than the second temperature region, separately from the step of adding the reactive dye; A dyeing method comprising the steps of:

2. The following steps: maintaining the temperature within the second temperature zone for a predetermined period of time; The dyeing method according to claim 1 , further comprising:

3. The dyeing method according to claim 1, wherein all of the mixture of the inorganic salt and the alkaline agent is added in portions in the third temperature zone.

4. The dyeing method according to claim 1, wherein all of the mixture of the inorganic salt and the alkaline agent is added in portions in the second temperature zone.

5. The divided addition is carried out three or more times and five or less times. When the total amount of the mixture of the inorganic salt and the alkaline agent is T (g), the amount added in the first stage is A (g), and the amount added in the second stage is B (g), the following formulas (1) to (3): 1 / 20×T≦A≦5 / 20×T…Formula (1) 1 / 20×T≦B≦7 / 20×T…Formula (2) A≦B…Formula (3) The dyeing method according to claim 1 or 2, wherein the above-mentioned condition is satisfied.

6. The dyeing method according to claim 1 or 2, wherein a total time period from the water supply to the end of the third temperature holding step is 100 minutes or less.

7. 7. The method of claim 6, wherein the total time period is 80 minutes or less.

8. 3. The dyeing method according to claim 1, wherein a dyeing reaction time period from the final stage of the divided addition to the end of the third temperature holding step is 20 minutes or more and 50 minutes or less.

9. 9. The method of claim 8, wherein the dyeing reaction time period is 40 minutes or more.

10. The dyeing method according to claim 1 or 2, wherein the third temperature is maintained at 60° C. or less.

11. 3. The dyeing method according to claim 1, wherein the time interval between the divided additions is from 5 minutes to 17 minutes.

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