A kind of Guangdong dark gauze dye and its preparation process

Abstract

The present invention belongs to the technical field of textile dyes, and particularly relates to a dye for Guangdong raw silk, the raw materials of which include the extract of Dioscorea cirrhosa, modifier A, emulsifier, ultraviolet shielding agent, coupling agent and solvent. The dye of the present invention has excellent adsorption capacity, anti-ultraviolet and antibacterial properties, and the antibacterial rate against Staphylococcus aureus and Enterobacter can reach over 99%. Moreover, it still maintains a high antibacterial activity after 20 washes, showing good wash fastness performance.

Description

Technical Field

[0001] The present invention belongs to the technical field of textile dyes, and particularly relates to a dye for xiangyunsha and a preparation process thereof. Background Art

[0002] Xiangyunsha is the only pure hand-made fabric dyed with natural dyes on silk fabrics among current textiles. It is made by repeatedly soaking and drying silk fabrics with the juice of Dioscorea cirrhosa for dozens of times, so that a thick red-brown pigment deposition layer is formed on the fabric surface. Then, natural river mud rich in iron is evenly applied to the darker front side of the fabric. After the reaction on the sandy land, the red-brown colloid on the front side of the fabric is transformed into a dark and shiny coating. Since xiangyunsha makes a rustling sound during daily activities, it was initially named "xiangyunsha" (rustling cloud yarn). Later, because the pronunciation of "rustling" and "fragrant" is similar, it was named "xiangyunsha".

[0003] As the only silk fabric hand-dyed with pure plant dyes in the current textile market, xiangyunsha has a dark and shiny front side and a brown back side. It is characterized by being fine, straight, smooth, cool and comfortable, and having the functions of sterilizing and repelling insects. It is hailed as "soft gold" in the textile industry and has a very large market demand. However, the production process of xiangyunsha is numerous, the production cycle is long, the cost is high, and it depends on natural factors such as light intensity, grassland, and river, which greatly reduces the production efficiency of xiangyunsha and cannot meet the market demand. Based on this, there is an urgent need to develop a dye for producing xiangyunsha. Summary of the Invention

[0004] In view of the problems existing in the prior art, the purpose of the present invention is to provide a xiangyunsha dye with excellent performance in all aspects to improve the production efficiency of xiangyunsha.

[0005] The present invention is realized through the following technical solutions:

[0006] A xiangyunsha dye, by weight, comprises the following raw materials:

[0007] 30 - 50 parts of Dioscorea cirrhosa extract

[0008] 5 - 10 parts of modifier A

[0009] 1 - 5 parts of emulsifier

[0010] 1 - 5 parts of ultraviolet shielding agent

[0011] 1 - 3 parts of coupling agent

[0012] 60 - 80 parts of solvent

[0013] The solvent is a mixed solvent of ethanol and water, wherein the weight percentage content of ethanol is 10 - 30%;

[0014] The preparation method of Dioscorea cirrhosa extract is:

[0015] Weigh a certain mass of Dioscorea cirrhosa powder, add an ethanol solution with a mass fraction of 60 - 80%, wherein the mass ratio of the Dioscorea cirrhosa powder to the ethanol solution is 1:(20 - 50), impregnate at 60 - 90°C, filter after cooling to room temperature, and evaporate the ethanol solvent under reduced pressure from the filtrate to obtain a Dioscorea cirrhosa extract;

[0016] The structure of the modifier A is as follows: .

[0017] In some embodiments, the coupling agent is selected from one or more of KH 550, KH 560, KH 570, KH 792, KH 791, DL - 602, and DL - 171.

[0018] In some embodiments, the coupling agent is selected from one or more of KH 550, KH 560, and KH 570.

[0019] In some embodiments, the ultraviolet shielding agent is selected from one or more of titanium dioxide, alumina, talcum powder, and calcium carbonate.

[0020] In some embodiments, the ultraviolet shielding agent is selected from one or more of titanium dioxide and alumina.

[0021] In some embodiments, the emulsifier is selected from one or more of Tween - 60, Tx - 10, triphenylvinylphenol polyoxyethylene ether, triphenylvinylphenol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and cashew phenol polyoxyethylene ether.

[0022] In some embodiments, the emulsifier is selected from one or more of Tween - 60, Tx - 10, and triphenylvinylphenol polyoxyethylene ether.

[0023] The present invention also provides a method for preparing the Guangdong raw silk fabric dye, comprising the following steps:

[0024] Step 1: Weigh a certain mass of Dioscorea cirrhosa powder, add an ethanol solution with a mass fraction of 60 - 80%, wherein the mass ratio of the Dioscorea cirrhosa powder to the ethanol solution is 1:(20 - 50), impregnate at 60 - 90°C, filter after cooling to room temperature, and evaporate the ethanol solvent under reduced pressure from the filtrate to obtain a Dioscorea cirrhosa extract, and store it refrigerated for later use;

[0025] Step 2: At room temperature, stir the Dioscorea cirrhosa extract, modifier A, emulsifier, ultraviolet shielding agent, coupling agent, and solvent in the above - mentioned mass ratio until they are evenly mixed to obtain the Guangdong raw silk fabric dye.

[0026] The present invention has achieved the following beneficial effects:

[0027] 1) The modifier A used in the present invention contains epoxy groups, which can react with the hydroxyl or amino groups on silk fibers in an alkaline environment, so that the silk fibers carry quaternary ammonium salt positive charges, which is conducive to the adsorption and dyeing of shuliang dyes, and thus has a high K / S value. In addition, the coupling agent used in the present invention can make the ultraviolet shielding agent powder uniformly dispersed in the solvent, prevent its agglomeration, enhance the binding ability between the ultraviolet shielding agent powder and the fabric, ensure the durability of the anti-ultraviolet finishing effect, and the modifier A contains triazine groups, which can be used synergistically with the ultraviolet shielding agent to exert excellent anti-ultraviolet performance.

[0028] 2) The fabric prepared with the dye of the present invention has excellent antibacterial properties against Escherichia coli and Staphylococcus aureus, and the antibacterial rate against Staphylococcus aureus and Enterobacter can reach more than 99%. And it still maintains a high antibacterial activity after 20 washes, and has good wash resistance.

[0029] 3) Since the present invention uses shuliang extract, the xiangyunsha also has the characteristics of mosquito prevention, insect prevention, strong waterproofness, easy to wash and dry, dark color and dirt resistance, light, thin, soft and not easy to wrinkle, which is very suitable for the climate in the south. Detailed implementation manners

[0030] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0031] The endpoints and any values of the ranges described in the present invention are not limited to the exact ranges or values. These ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, between the endpoint values of each range, between the endpoint values of each range and a single point value, and between single point values can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed herein.

[0032] The structure of the modifier A used in Examples 1-3 is: , prepared by referring to the method disclosed in CN104086512B, specifically as follows:

[0033] Add dimethylamine solution to a reactor equipped with a reflux condenser, then slowly drop epichlorohydrin (1.0 mol) at room temperature, and stir the reaction for 5 hours after the drop is complete. After distilling off the water, slowly drop cyanuric chloride (1.0 mol) into the reactor at 5°C, and continue to stir the reaction for 3 hours after the drop is complete. Then, distill the obtained product under reduced pressure to remove the residual unreacted compounds and by-products, control the system temperature at about 30°C and the pressure at 4Kpa, and collect the volatile substances with a dry ice collector until the product solution is concentrated into a thick slurry, and the above-mentioned modifier A is obtained.

[0034] Example 1

[0035] A Xiangyunsha dye, comprising the following raw materials in parts by weight:

[0036] Dioscorea extract 50 parts

[0037] Modifier A 10 parts

[0038] Emulsifier Tween-60 3 parts

[0039] UV shielding agent titanium dioxide 3 parts

[0040] Coupling agent KH-550 1 part

[0041] 60 parts of solvent

[0042] The solvent is a mixed solvent of ethanol and water, wherein the mass percentage of ethanol is 20%;

[0043] The preparation method of the Xiangyunsha dye comprises the following steps:

[0044] Step 1: Weigh a certain mass of Dioscorea scoparia powder, add a 60% ethanol solution by mass, wherein the mass ratio of Dioscorea scoparia powder to 60% ethanol solution is 1:20, soak at 60°C for 5 hours, cool to room temperature and filter, evaporate the filtrate under reduced pressure to remove the ethanol solvent to obtain Dioscorea scoparia extract, and refrigerate below 5°C for later use.

[0045] Step 2: At room temperature, stir the yam extract, modifier A, emulsifier, UV shielding agent, coupling agent and solvent according to the above mass ratio until they are uniformly mixed to obtain Xiangyunsha dye.

[0046] Example 2

[0047] A Xiangyunsha dye, comprising the following raw materials in parts by weight:

[0048] 40 parts of Dioscorea extract

[0049] Modifier A 8 parts

[0050] Emulsifier Tx-10 5 parts

[0051] 2 parts of ultraviolet screening agent alumina

[0052] 2 parts of coupling agent KH-570

[0053] 80 parts of solvent

[0054] The solvent is a mixed solvent of ethanol and water, wherein the mass percentage of ethanol is 30%;

[0055] The preparation method of the said Guangdong gauze dye comprises the following steps:

[0056] Step 1: Weigh a certain mass of Dioscorea cirrhosa powder, add an ethanol solution with a mass fraction of 70%, wherein the mass ratio of Dioscorea cirrhosa powder to the 70% ethanol solution is 1:30, soak at 70 °C for 4 h, filter after cooling to room temperature, and remove the ethanol solvent from the filtrate by reduced pressure evaporation to obtain Dioscorea cirrhosa extract, and refrigerate it for standby at a temperature below 5 °C.

[0057] Step 2: At room temperature, stir the Dioscorea cirrhosa extract, modifier A, emulsifier, ultraviolet screening agent, coupling agent and solvent evenly according to the above mass ratio to obtain the Guangdong gauze dye.

[0058] Example 3

[0059] A Guangdong gauze dye, by weight, comprises the following raw materials:

[0060] 50 parts of Dioscorea cirrhosa extract

[0061] 8 parts of modifier A

[0062] 4 parts of emulsifier triphenylvinylphenol polyoxyethylene ether

[0063] 3 parts of ultraviolet screening agent titanium dioxide

[0064] 1 part of coupling agent KH-560

[0065] 70 parts of solvent

[0066] The solvent is a mixed solvent of ethanol and water, wherein the mass percentage of ethanol is 30%;

[0067] The preparation method of the said Guangdong gauze dye comprises the following steps:

[0068] Step 1: Weigh a certain mass of Dioscorea cirrhosa powder, add an ethanol solution with a mass fraction of 80%, wherein the mass ratio of Dioscorea cirrhosa powder to the 80% ethanol solution is 1:20, soak at 60 °C for 5 h, filter after cooling to room temperature, and remove the ethanol solvent from the filtrate by reduced pressure evaporation to obtain Dioscorea cirrhosa extract, and refrigerate it for standby at a temperature below 5 °C.

[0069] Step 2: At room temperature, stir the Dioscorea cirrhosa extract, modifier A, emulsifier, ultraviolet shielding agent, coupling agent and solvent according to the above mass ratio until they are evenly mixed to obtain the Guangdong gauze dye.

[0070] Comparative Example 1

[0071] On the basis of Example 1, modifier A was omitted, and the specific operation was as follows:

[0072] A Guangdong gauze dye, by weight, includes the following raw materials:

[0073] Dioscorea cirrhosa extract 50 parts

[0074] Emulsifier Tween-60 3 parts

[0075] Ultraviolet shielding agent titanium dioxide 3 parts

[0076] Coupling agent KH-550 1 part

[0077] Solvent 60 parts

[0078] The solvent is a mixed solvent of ethanol and water, and the mass percentage content of ethanol is 20%;

[0079] The preparation method of the Guangdong gauze dye includes the following steps:

[0080] Step 1: Weigh a certain mass of Dioscorea cirrhosa powder, add an ethanol solution with a mass fraction of 60%, wherein the mass ratio of Dioscorea cirrhosa powder to the 60% ethanol solution is 1:20, impregnate at 60 °C for 5 h, filter after cooling to room temperature, and evaporate the ethanol solvent under reduced pressure from the filtrate to obtain the Dioscorea cirrhosa extract, and store it refrigerated below 5 °C for later use.

[0081] Step 2: At room temperature, stir the Dioscorea cirrhosa extract, emulsifier, ultraviolet shielding agent, coupling agent and solvent according to the above mass ratio until they are evenly mixed to obtain the Guangdong gauze dye.

[0082] Comparative Example 2

[0083] On the basis of Example 1, modifier A was replaced with modifier B , and other conditions were the same as in Example 1.

[0084] Antibacterial performance test:

[0085] The Guangdong gauze dyes of Examples 1-3 and Comparative Examples 1-2 were used for dyeing silk fabrics, and the dyeing steps were as follows:

[0086] Step S1: Immerse 19 MM silk habotai in 30 times its mass of the Guangdong gauze dye, and use Na 2 CO 3Adjust the pH value of the dyeing bath to 9, heat it up to 60 °C and keep it at a constant temperature for 2 h;

[0087] Step S2: Treat the silk habotai dyed in Step S1 in a treatment bath of ferrous sulfate at 80 °C and 20% for 30 min, then wash it with soap, wash it with water, and dry it to obtain the xiangyunsha fabric.

[0088] Measure the ultraviolet resistance, dyeing K / S value, and antibacterial performance of the above-mentioned xiangyunsha fabric. The measurement methods are as follows:

[0089] 1) Ultraviolet resistance performance test

[0090] Conduct the test according to GB / T 18830-2009 "Evaluation of Ultraviolet Resistance Performance of Textiles". Use a UV-2000F type textile ultraviolet resistance factor tester to measure the UPF value of the fabric. Take any 3 points for testing and take the average value.

[0091] 2) Dyeing K / S value test

[0092] The dyeing K / S value is measured with an SF600+ type computer color measuring and matching instrument according to the operating rules. Each sample is tested three times in different areas, and the average value is taken as the dyeing K / S value. Test conditions: D65 light source, 10° viewing angle.

[0093] 3) Antibacterial performance test

[0094] Conduct the antibacterial test according to the standard of GB / T 20944.3-2008.

[0095] The results are shown in Table 1 and Table 2.

[0096] Table 1 Test results of ultraviolet resistance UPF value and K / S value

[0097]

[0098] Table 2 Antibacterial performance test

[0099]

[0100] As can be seen from Table 1, the fabric prepared with the dye of the present invention has excellent ultraviolet resistance and dye adsorption properties. The main reasons are as follows: First, the modifier A used in the present invention contains epoxy groups, which can react with the hydroxyl or amino groups on the silk fiber in an alkaline environment, so that the silk fiber is positively charged with quaternary ammonium salt, which is beneficial to the adsorption and dyeing of the shiliang dye, and thus has a high K / S value; In addition, the coupling agent used in the present invention can make the ultraviolet shielding agent powder uniformly dispersed in the solvent, prevent its agglomeration, enhance the binding ability between the ultraviolet shielding agent powder and the fabric, ensure the durability of the anti-ultraviolet finishing effect, and the modifier A contains triazine groups, which can be used synergistically with the ultraviolet shielding agent to exhibit excellent ultraviolet resistance.

[0101] As can be seen from Table 2, the fabric prepared with the dye of the present invention has excellent antibacterial properties against Escherichia coli and Staphylococcus aureus, and the antibacterial rates against Staphylococcus aureus and Enterobacter can reach over 99%. And after 20 washes, it still maintains a high antibacterial activity and has good wash resistance. The main reasons are that the quaternary ammonium salt and triazine groups contained in the modifier A both have certain antibacterial properties, which can be connected to the silk fiber through chemical bonds and have high stability, and the modifier A can be used synergistically with some antibacterial active ingredients in the shiliang extract to exhibit excellent antibacterial properties.

[0102] In addition, since the present invention uses the shiliang extract, the xiangyunsha also has the characteristics of mosquito prevention, insect prevention, strong waterproofness, easy washing and drying, dark color and dirt resistance, lightness, softness and non-crease, which is very suitable for the climate in the south.

[0103] The above embodiments are only examples clearly described and not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. And the obvious changes or modifications thus derived are still within the protection scope of the present invention.

Claims

1. A Xiangyunsha dye, comprising the following raw materials by weight: 30-50 parts of Dioscorea scoparia extract; Modifier A 5-10 parts; Emulsifier 1~5 parts; 1~5 parts of UV shielding agent; 1~3 parts of coupling agent; 60-80 parts of solvent; The solvent is a mixed solvent of ethanol and water, wherein the weight percentage of ethanol is 10-30%; The preparation method of the yam extract is as follows: Weigh a certain amount of Dioscorea powder and add 60-80% ethanol solution, where: The mass ratio of yam powder to ethanol solution is 1:(20-50), the mixture is immersed at 60-90°C, cooled to room temperature and filtered, and the filtrate is evaporated under reduced pressure to remove the ethanol solvent to obtain yam extract; The structure of the modifier A is: ; The coupling agent is selected from one or more of KH-550, KH-560, and KH-570; The ultraviolet shielding agent is selected from one or more of titanium dioxide and aluminum oxide; The emulsifier is selected from one or more of Tween-60, Tx-10, and tristyrylphenol polyoxyethylene ether.

2. A method for preparing the Xiangyunsha dye according to claim 1, comprising the following steps: Step 1: Weigh a certain amount of Dioscorea powder and add 60-80% ethanol solution, where: The mass ratio of Dioscorea scoparia powder to ethanol solution is 1:(20-50), the mixture is immersed at 60-90°C, cooled to room temperature and filtered, the filtrate is evaporated under reduced pressure to remove the ethanol solvent to obtain Dioscorea scoparia extract, and the extract is refrigerated for later use; Step 2: At room temperature, stir the yam extract, modifier A, emulsifier, UV shielding agent, coupling agent and solvent according to the above mass ratio until they are uniformly mixed to obtain Xiangyunsha dye.

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