KR19990065741A - Textile dyeing method using ocher powder - Google Patents

Abstract

The present invention relates to a method for dyeing fibers using ocher powder, and in particular, by increasing the adsorption rate of ocher particles to cotton fibers and by firmly fixing the ocher particles adsorbed inside the fibers using a cotton fiber fixing agent. The present invention relates to a method of dyeing fibers using loess powder having a high washing fastness corresponding to a general dyeing product.

The present invention comprises the steps of preparing a high-density ocher dye containing only the atomized ocher particles through the sequential small particle size after diluting / stirring the ocher in water, and the raw material to be dyed to increase the adsorption rate of the ocher particles After pretreatment of the support stage, the pretreatment step of pretreatment to a cationic state, and the high concentration of ocher dye diluted in water to 10-30% owf, and then the pretreated raw supporter is added to the dyeing tank and dyed at a temperature between 100-130 ° C. After performing the dyeing step of cooling and hot water after cooling, characterized in that it comprises a post-treatment step of fixing the adsorbed ocher particles by treating the ocher dyed fabric with a cotton fiber fixing agent.

Description

Textile dyeing method using ocher powder

The present invention relates to a method for dyeing fibers using ocher powder, and in particular, by increasing the adsorption rate of ocher particles to cotton fibers and by firmly fixing the ocher particles adsorbed inside the fibers using a cotton fiber fixing agent. The present invention relates to a method of dyeing fibers using loess powder having a high washing fastness corresponding to a general dyeing product.

Ocher is widely scattered around us, and therefore, our ancestors have traditionally worn cotton cloth by dyeing cotton cloth in the state of dispersing it in water.

The mineral composition of ocher is generally composed of 40-80% quartz, 10-20% feldspar and mica, 5-35% carbonate mineral, and 2-5% silt, where silt is made of chromite, inhee, It is composed of heavy minerals such as biotite, chlorite, citrine, verdite, garnet, arsenite, rutile, quartzite, cruciate, tourmaline, and zircon.

Looking at the chemical composition of the loess as described above, silica (SiO ₂ ) 50-60%, alumina (Al ₂ O ₃ ) 8-12%, trivalent iron oxide (fe ₂ O ₃ ) 2-4%, divalent iron oxide ( feO) 0.8-1.1%, calcium oxide (CaO) 4-16%, magnesium oxide (MgO) 2-6%, and about 0.5% titanium oxide (TiO ₂ ) and manganese oxide (MnO) is generally composed The water content is 10-15% and the porosity is 50-55%, but the porosity tends to decrease with increasing water content.

In addition to the minerals mentioned above, ocher has various kinds of enzymes which are organic substances. For example, decay of catalase, diphenol oxidase, sugar-degrading saccharase, and protein that are known to be indicative of soil oxidative power and remove hydrogen peroxide (H ₂ O ₂ ), which causes toxins to organisms It is known to contain a protease or the like which is an enzyme.

Recently, ocher emits far-infrared rays which are beneficial to human body by the action of the above minerals, and many uses such as water quality improvement effect, treatment effect and cosmetic effect have been found by enzyme action. It is being used as a situation.

On the other hand, the conventional ocher dyeing method was just a basic dyeing to the yellow soil in order to prevent the burn easily stained when the common people in the times when dyes are usually processed by clothing as a garment. In this case, the dyeing condition was severely dyed due to stains and discoloration due to washing.

Therefore, the conventional ocher dyeing method has a qualitative level with the concept of 'dyeing', which is a dyeing method using a conventional dye, that is, it does not change color even if it is worn / washed many times by attaching the dye to the fiber and fixing it. It is different. As a result, inexpensive chemical dyes and dyeing techniques have been developed today, and the conventional ocher dyeing method has disappeared.

Recently, in order to provide a dyeing effect that does not cause discoloration and staining, which is a problem of the conventional ocher dyeing method, a method of dyeing fibers using ocher powder has been proposed in Korean Patent Publication No. 97-62180.

In the dyeing method disclosed in the above-mentioned Patent Publication, the ocher powder is separated, and only the fine ocher powder having a particle diameter of 0.005 mm or less is collected and suspended in water to prepare an ocher salt bath, and the ocher salt bath is heated to maintain a temperature of the salt bath at 90 ° C. After maintaining the above, the fiber is immersed and stirred for 5-10 minutes, followed by ocher dyeing, and then the dried fiber is picked up and dried and washed.

However, in the conventional dyeing method using ocher powder, the results of the test of the performance of the ocher dyed fiber showed that the change of washing fastness according to Korean Industrial Standard KS K 0430 has a level of 2-3. This is considered to be a dyeing method that is difficult to commercialize, considering that the level of change in washing fastness required for general cotton fiber products is about 4th grade.

Therefore, the inventors have analyzed the prior art precisely, and thus, the prior art controls the particle size of the ocher powder, increases the dyeing temperature, and also removes the ocher powder adsorbed on the fiber surface by the natural washing method. It can be seen that only the 'physical' method is used, and furthermore, since the chemical properties and physical structure of the ocher particles have no affinity with cotton fibers, the physical fastness of the dyeing process is basically equivalent to that of general dyeing products. It was recognized that it was impossible to obtain a product with

Accordingly, the present inventors have conducted a lot of research to solve the problems of the prior art, and found that the ocher particles are weakly electrically negatively charged (-) to increase the adsorption rate of the ocher particles by cationic pretreatment of the fabric. By adhering the adsorbed ocher particles chemically with a cotton fiber fixing agent, the ocher dyeing method, which can drastically increase the degree of change in washing fastness, has been completed.

Therefore, the present invention has been made in view of the problems of the prior art, the purpose of which is to increase the adsorption rate of the ocher particles to the cotton fiber and at the same time to firmly adhere the ocher particles adsorbed inside the fiber using a cotton fiber fixing agent. The present invention provides a method for dyeing fibers using loess powder having a high washing fastness corresponding to a general dyeing product by zooming.

In order to achieve the above object, the present invention comprises the steps of preparing a high concentration of ocher dye containing only the ocher particles in the atomized state after the dilution / stirring of the ocher in water and sequential small particle size, and the ocher particles The pretreatment step of refining the live support stage to be dyed in order to increase the adsorption rate of the pre-treatment to a cationic state, and diluting the high concentration ocher dye to 10-30% owf in water, and then put the pretreated raw support stage into the dyeing tank 100 Ocher, characterized in that consisting of a dyeing step of performing a dyeing at a temperature between -130 ℃ and cooling after hot water, and a post-treatment step of fixing the adsorbed ocher particles by treating the ocher dyed fabric with a cotton fiber fixing agent. It provides a method of dyeing fibers using powder.

Hereinafter, the present invention will be described in more detail.

The present invention relates to a method for dyeing fibers using ocher powder, which can significantly increase the adsorption rate of ocher dyes and at the same time have good washing fastness that hardly changes even when the adsorbed dye undergoes washing. Specifically, it is as follows.

In detail the preparation step of the high concentration ocher dye, first remove the collected ocher by picking a tree root and a large boulder, etc., loosened in water at a dilution ratio of about 15 wt.% And stirred for at least about 60 minutes.

The well-stirred ocher suspension is then removed using a 150 μm mesh standard mesh to remove small grass roots, sand and the like. Subsequently, the ocher solution having fine ocher particles was collected by filtering the ocher suspension while sequentially lowering the mesh size to, for example, 106, 75, 63, 53, and 45 μm, and the obtained ocher suspension was subjected to an ultrasonic homogenizer. To prepare a high-concentration ocher dye through ultrasonic grinding so that the ocher particles are atomized by using. At this time, measure the pure concentration of the ocher dye prepared to easily match the exact dilution ratio in the dyeing step.

On the other hand, the pretreatment step of the live support stage to increase the adsorption rate of the ocher particles is made as follows. First, the raw support for cotton fibers is used as a scouring agent for cotton fibers, for example, the liquid ratio between surfactants containing caustic soda (NaOH) is refined in a scouring bath, which is preferably set at about 1:10 to remove fats and oils in the fibers. Remove

Subsequently, sufficient water washing is performed to remove impurities and residual surfactant in the fiber, and preferably, about two times of boiling water treatment may be performed.

After neutralizing the alkaline fabric according to the above-mentioned refining treatment, 5 wt.% Of cationic agent (cationic agent) is added to adjust pH to 4-6 weak acidity, and then immersed for about 30 minutes at 70 ° C. It is prepared in such a state that ocher dye can be easily adsorbed to the fabric to be dyed by dehydration and drying after treatment.

This cationization of the fabric to be dyed can greatly increase the adsorption rate of the ocher particles in the fiber during the ocher dyeing step because the ocher particles have a very weak negative potential.

Subsequently, the dyeing step of the ocher is homogenized by diluting the high-concentration ocher dye prepared in water in the range of 10-30% owf (on the weight of fiber) and treating it with ultrasonic waves for about 60 minutes, and pretreating the pretreated fabric with liquid ratio of about 1 While operating at a ratio of: 10, add dispersant and slowly add ocher dye for about 20 minutes to ensure uniformity.

The temperature is then raised to a temperature of 100-130 ° C. at a rate of 1.5 ° C./min, dyed for at least 10 minutes under high pressure, cooled to about 70 ° C., and then subjected to overflow washing. Then, rinse 5-6 times with hot water in 80 ℃ heated water until the salt solution is clear.

Finally, the post-treatment step for fixing the ocher particles is first heated and then added with a soaping agent (Soaping) to soak for 20 minutes at about 98 ℃ and remove the unadsorbed ocher dye by boiling water and hot water.

Then, after adding 3wt.% Cotton fiber fixing agent, it is treated at about 40 ℃ for 20 minutes, and the fabric is taken out and dehydrated and dried. The yellow soil dye adsorbed on the fiber is firmly fixed so that washing fastness corresponding to dyeing product using general reactive dye is fixed. A loess dyed product having is obtained.

On the other hand 10% o.w.f. When diluted with water below, the concentration after dyeing cannot be obtained to the desired level, and 30% o.w.f. In case of abnormality, only the amount of dye is wasted but the concentration after dyeing does not increase any more, so the dilution concentration of ocher dye is 10-30% o.w.f. It is preferable to set between.

In addition, the dyeing temperature is suitable in the range of 100-130 ℃. The reason is that when the temperature is less than 100 ° C., the leveling property is inferior, and when the temperature is 130 ° C. or more, it does not affect the quality of the dyeing product, but an expensive special facility is required to maintain the high pressure.

As described above, in the present invention, by increasing the adsorption rate of the ocher particles by cationic pretreatment of the fabric to be dyed in consideration of the properties of the ocher particles and chemically fixing the adsorbed ocher particles with a cotton fiber fixing agent, the degree of change in washing fastness is remarkable. I can pull it up.

Hereinafter, the present invention described above will be described in detail with reference to Examples, but the present invention is not limited by Examples.

Example 1

The collected ocher was removed by selecting a tree root and a large boulder, and then, dissolved in water at a dilution ratio of about 15 wt.%, And left to stir for 60 minutes. The well-stirred ocher suspension was then removed using small sized grass roots, sand, etc. using a standard 150 μm mesh net. Subsequently, the ocher suspension having fine ocher particles was collected by filtering the ocher suspension while sequentially lowering the mesh size to 106, 75, 63, 53, and 45 μm, and the obtained ocher suspension was ground by an ultrasonic homogenizer to obtain a high concentration. An ocher dye was prepared. At this time, the pure concentration of the prepared ocher dye was measured.

Meanwhile, the flat knit fabric for knits knitted using CM40s cotton yarn was refined for 60 minutes at 98 ° C. in a refining bath in which the liquid ratio between nonionic surfactants including caustic soda (NaOH) was set to 1:10. Water washing was performed sufficiently. Thereafter, after neutralization, 5 wt.% Of ALCOfIX 2206 was added as a cationic agent (cationic agent) to adjust the pH to 5, and the fabric was dyed by immersion at about 70 ° C. for 30 minutes, and then dried to prepare a fabric to be dyed.

After diluting the high-concentration ocher dye in water at 25% owf and homogenizing it by ultrasonic treatment for 60 minutes, the pretreated fabric was run at a liquid ratio of 1:10, and 1 g / ℓ was added using Setamol WS as a dispersant. Slowly add over 20 minutes. Thereafter, the temperature was raised to 110 ° C. at a rate of 1.5 ° C./min, dyed for 40 minutes under high pressure, cooled to 70 ° C., and overflow washing was performed. Subsequently, hot water washing was performed 5 times with 80 degreeC boiling water.

Finally, 2 g / l of nonion anti-soaping agent (Liponox NCI) was added to the mixture for 20 minutes at 98 ° C., and the unsorbed ocher dye was removed by boiling water and hot water. Thereafter, 3 wt.% Of Protex GRD was added as a cotton fiber fixing agent, and then treated at 40 ° C. for 20 minutes, and the fabric was taken out, dehydrated and dried to dye the cotton fiber fabric of Example 1.

In this case, in order to check the optimal size condition of the ocher particles in the dyeing method of Example 1, the dyeing process is carried out while changing only the size of the ocher particles to four kinds, and the color fastness (discoloration) and the concentration after the treatment of the dyed fabric are changed. After the test, the results are shown in Table 1 below. In this case, however, dyeing was performed without undergoing a pretreatment process of cationic cation.

Size Conditions of Ocher Particles Particle size Treatment method Post-Dyeing Concentration Fastness to Laundry (varies) ⁽¹⁾ Comparative Example 1 Remove only impurities ○ 2-3 Comparative Example 2 150μm or less Use standard mesh ◎ 2-3 Comparative Example 3 40μm or less Use standard mesh ◎ 3 to 4 Comparative Example 4 10μm or less Standard mesh + powder grinder △ 3 to 4

In Table 1, ◎: very dark, ○: dark, △: weak.

The powder mill used in Comparative Example 4 described above is a dry mill.

As a result of the experiment, it was found that an example of uniformly collecting ocher particles with a particle size of 40 μm or less by using a standard network yielded the best results in terms of concentration and washing fastness. However, when the pretreatment process of cationizing the fabric according to the present invention irrespective of the size of the particles, the fastness of washing was similarly obtained to about 4 products, and only slightly after the dyeing, the above-mentioned difference occurred. .

In addition, in order to confirm the optimum PH value of the cationic agent for pretreatment, that is, cationic, of the fabric to be dyed in the dyeing method of Example 1 described above, the dyeing process is performed while changing only the PH value into three types of weak acid, neutral, and weak alkali. After washing the wash fastness (discoloration) and the post-dyeing concentration for the dyed fabric is shown in Table 2 below.

PH condition of the cationic agent PH condition Post-Dyeing Concentration Wash fastness (variation) Inventive Example PH 4 ~ 6 ◎ 4 Comparative Example 5 PH 6-8 ○ 3 to 4 Comparative Example 6 PH 8-10 △ 2-3

In Table 2,?: Very thick,?: Dark,?: Weak.

As a result of the experiment, it was found that the present invention, which treated the PH condition with weak acidity when using the cationic agent, showed the best results in terms of concentration and wash fastness (discoloration) after dyeing. This is thought to be a phenomenon because the ocher dye has a weak negative potential.

In addition, in order to confirm the optimum conditions for the dyeing temperature at the time of ocher dyeing in the dyeing method of Example 1, the dyeing temperature was changed to only four types to test the dyeing concentration and leveling degree of the dyed fabric. The results are shown in Table 3 below.

Dyeing temperature condition Dyeing temperature Post-Dyeing Concentration Uniformity Remarks Comparative Example 7 60 ℃ or less ○ △ Comparative Example 8 60 ℃ -100 ℃ ◎ ○ Inventive Example 1 100 ℃ ~ 120 ℃ ◎ ◎ High pressure vessel required Inventive Example 2 120 ℃ or more ◎ ◎ High pressure vessel required

○ At the dyeing concentrations in Table 3: Normal, ◎: Dark

In addition, in the level of the bactericidal properties of Table 3,?: Tends to be disproportionate, ○: normal, and?

As a result of the experiment, the dyeing temperature is more than 100 ℃ dyeing is advantageous in the homogeneous measurement, it can be seen that there is no significant difference in the temperature above. However, in order to maintain a temperature of 100 ° C or higher, a container capable of applying pressure under a sealed container is required.

Example 2

Dyeing was carried out in the same manner as in Example 1 except that the pretreatment for cationization of the fabric was set to 6, the dilution ratio of the high concentration of ocher dye to water was adjusted to 12% owf, and the dyeing temperature was 130 ° C. The dyeing in the state set to measure the washing fastness and friction fastness and the results are shown in Table 4 below.

Conventional Example 1

According to the method disclosed in the above-described Korean Patent Publication No. 97-62180, dyeing is performed without carrying out a pretreatment process for cationizing a fabric and a post-treatment process for fixing ocher dyes, and washing fastness and friction of the dyed fabric. The fastness was tested and the test results are shown in Table 4 below.

Comparative Example 9

In the dyeing method of Example 1, only the pretreatment step of cationizing the cotton fiber fabric is omitted, and the test results of the laundry fastness and the friction fastness of the dyed fabric are shown in Table 4 below.

Comparative Example 10

In the dyeing method of Example 1, only the post-treatment step of fixing the ocher dye of the dyed fabric is omitted, and the test results of the laundry fastness and the friction fastness of the dyed fabric are shown in Table 4 below. It was.

The wash fastness of the dyed fabric was tested according to Korean Industrial Standard KSK-430 (A-1), and the friction fastness was tested according to Korean Industrial Standard KSK-650.

Sample name Color fastness Color fastness Disguise pollution key Wet Example 1 4 to 5 4 to 5 4 to 5 4 to 5 Example 2 4 to 5 4 to 5 4 to 5 4 to 5 Conventional Example 1 2-3 4 to 5 3 2 Comparative Example 9 3 to 4 4 to 5 3 to 4 3 Comparative Example 10 3 to 4 4 to 5 3 3

In case of dyeing using ocher dye having a particle size of 0.005mm according to the conventional example 1, there is no pretreatment to increase the adsorption rate of ocher, so that the adsorption rate of ocher is lowered and the adsorbed ocher dye has no post-treatment to fix it. As a result, the change was greatly progressed, and the washing fastness was found to reach a very low level of 2-3, which is not practical.

In addition, when the experimental results of Comparative Example 9 and Comparative Example 10 were judged, it was shown that the washing fastness was greatly affected even if one of the pretreatment for increasing the adsorption rate of the loess or the post-treatment for fixing the adsorbed ocher dye were omitted. .

On the contrary, when the dyeing is performed by performing both pretreatment to increase the adsorption rate of loess and post-treatment to fix the adsorbed ocher dye, as in Examples 1 and 2, both washing fastness and friction fastness can be commercialized. The level was -5.

In addition, the results of the above experiment showed that the contamination of the washing fastnesses was not a problem in both the Examples and Comparative Examples according to the present invention. These results indicate that the ocher particles do not have affinity with the original fiber, so that sufficient post-washing after dyeing is not a problem.

On the other hand, the ocher powder having a particle size of 0.005 mm or less obtained when preparing the ocher powder by the conventional defensive method or the separation method by wind according to the conventional example 1 can obtain only 3-5% and 95-97% It was found that the loess has a problem that the processing cost of loess dye is increased by the loss treatment.

However, when the preparation method of the ocher dye according to the present invention showed about 30% of the ocher refining rate, the manufacturing cost of the ocher dye could be greatly reduced as compared with the conventional one, which is the adsorption rate of the ocher, the concentration after dyeing and the wash fastness. We believe it is helping to increase the

Although not shown in the table, the results of the experiment showed that cotton products had better dyeing results than synthetic fibers, and in particular, cotton fabrics with elasticity had better dyeing results than cotton fabrics.

As described above, in the present invention, by increasing the adsorption rate of the ocher particles by cationic pretreatment of the fabric to be dyed in consideration of the properties of the ocher particles and chemically fixing the adsorbed ocher particles with a cotton fiber fixing agent, the degree of change in washing fastness is remarkable. I can pull it up.

In the above, the present invention has been illustrated and described with reference to specific preferred embodiments, but the present invention is not limited to the above-described embodiments and is not limited to the spirit of the present invention. Various changes and modifications can be made by those who have

Claims (5)

Diluting / stirring the ocher in water and then preparing a high concentration of the ocher dye containing only the atomized ocher particles through the sequential small particle size selection process, A pretreatment step of refining the live support stage to be dyed to increase the adsorption rate of the ocher particles and then pretreating it to a cationic state; After diluting the high concentration ocher dye in water at 10-30% o.w.f. The dyeing method of the fiber using the ocher powder, characterized in that the ocher-dyed fabric is treated with a cotton fiber fixing agent to fix the adsorbed ocher particles. The method of claim 1, wherein the pretreatment step is a dyeing method of the fiber using ocher powder, characterized in that to adjust the fabric to be dyed using a cationic agent in a slightly acidic state. The method according to claim 1 or 2, wherein the pretreatment step includes a refining step of removing oils and other impurities to the fabric; After washing with water, the dyeing method of the fiber using ocher powder, characterized in that it further comprises the step of neutralizing. The method of claim 1, wherein the post-treatment step removes the unadsorbed ocher dye by high temperature soaping and hot water, adds about 3 wt. A method for dyeing fibers using ocher powder, characterized in that. The method of claim 1, wherein the step of preparing the ocher dye dyeing method of the fiber using ocher powder, characterized in that it further comprises a homogenization step using ultrasonic waves.