CN112458771B - Deepening agent for nylon fabric and preparation method thereof - Google Patents
Deepening agent for nylon fabric and preparation method thereof Download PDFInfo
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- CN112458771B CN112458771B CN202011256123.3A CN202011256123A CN112458771B CN 112458771 B CN112458771 B CN 112458771B CN 202011256123 A CN202011256123 A CN 202011256123A CN 112458771 B CN112458771 B CN 112458771B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/24—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen halogen-containing groups
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a deepening agent for nylon fabric and a preparation method thereof. Organic dicarboxylic acid, epoxy double-end socket, polyether amine, octamethylcyclotetrasiloxane and trifluoropropylmethyl cyclotrisiloxane are used as raw materials to synthesize the deepening agent. The fluorine-containing polysiloxane chain segment in the molecular structure of the deepening agent provided by the invention can effectively reduce the light reflection amount of the surface of the finished nylon fabric, so that the apparent depth of the nylon fabric is increased, and meanwhile, the polyether chain segment in the molecular structure can improve the hydrophilic performance of the finished nylon fabric. In addition, according to the principle that the structures are similar and compatible, a polyamide chain segment in the molecular structure of the deepening agent can form eutectic with a molecular chain segment of nylon (polyamide fiber) under the condition of high-temperature baking, and the finished nylon fabric has a washable deepening effect.
Description
Technical Field
The invention relates to the technical field of synthesis of printing and dyeing auxiliaries, and particularly relates to a deepening agent for nylon fabrics and a preparation method thereof.
Background
With the continuous improvement of living standard, people have higher and higher requirements on dark fabrics, but are restricted by the dye uptake and the dye fastness in fiber dyeing balance, and when the fabrics are dyed in dark colors, a large amount of unfixed dye exists on the surfaces of the fabrics, so that the fabrics are not dark in dark colors and insufficient in color fastness, a large amount of printing and dyeing wastewater can be generated after dyeing, and with the continuous improvement of environmental protection requirements, the cost for treating the printing and dyeing wastewater is higher and higher. Therefore, the deep dyeing method has important significance for reducing the using amount of the dye and the production cost by using the deep dyeing agent.
In general, a deepening agent is a resin with low refractive index, and after finishing, a film is formed on the surface of a fiber, so that the reflection amount of light on the surface of the fiber is changed, and the apparent depth of the fabric color is increased. Common resins with low refractive index include fluorine resins, silicone resins, and the like. The fluororesin has low refractive index, good deepening effect and higher cost; the silicone resin is relatively low in cost, but the deepening effect is not ideal enough. Therefore, the development of a deepening agent with good effect and relatively low cost is of great significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the deepening agent capable of effectively improving the deepening effect of the nylon fabric dyeing and reducing the dyeing cost and the preparation method thereof.
In order to achieve the aim, the technical scheme adopted by the invention provides a preparation method of a deepening agent for nylon fabric, which comprises the following steps:
(1) adding 20 parts by mass of polyether amine and 15-20 parts by mass of organic dibasic acid into a first reaction vessel with a stirrer and a condensation reflux device, opening the condensation reflux device and the stirrer, adding sodium hypophosphite accounting for 1.5-2% of the total mass of the reaction monomers, heating to 175 ℃, adding triphenyl phosphite accounting for 1.5-2% of the total mass of the reaction monomers, continuously heating to 220-230 ℃, and carrying out heat preservation reaction for 1-2 hours to obtain an intermediate product I;
(2) adding 15 parts of octamethylcyclotetrasiloxane, 5-15 parts of trifluoropropylmethylcyclotrisiloxane and 2-3 parts of epoxy double-seal head into a second reaction container with a stirrer, starting the stirrer, heating to 70-75 ℃, adding tetramethylammonium hydroxide accounting for 0.08-0.1% of the total mass of the reaction monomers, continuing heating to 90-100 ℃, and carrying out heat preservation reaction for 5-6 hours to obtain an intermediate product II;
(3) and adding 30 parts of the intermediate product II, 30-60 parts of the intermediate product I and 25-60 parts of isopropanol into a third reaction vessel provided with a stirrer and a condensation reflux device, starting the stirrer and the condensation reflux device, heating to 75-80 ℃, preserving heat, reacting for 4 hours, and then decompressing to remove the isopropanol solvent to obtain the deepening agent for the nylon fabric.
One preferred embodiment of the present invention is: the number average molecular weight of the polyether amine in the step (1) is 400 or 600; the organic dibasic acid is one of adipic acid, azelaic acid and sebacic acid.
The technical scheme of the invention also comprises the deepening agent for the nylon fabric, which is obtained by the preparation method.
The deepening agent provided by the invention, an emulsifier and water are prepared into emulsion, and the nylon fabric is finished.
The principle of the invention is as follows: the introduction of fluorine-containing groups into the organic silicon molecular chain segment not only can enhance the deepening effect of the organic silicon, but also can reduce the cost compared with the pure fluorine-containing resin. The fluorine-containing polysiloxane chain segment in the molecular structure of the deepening agent can effectively reduce the light reflection amount of the surface of the finished nylon fabric, so that the apparent depth of the nylon fabric is increased, and meanwhile, the polyether chain segment in the molecular structure can improve the hydrophilic performance of the finished nylon fabric. In addition, according to the principle that the structure is similar and compatible, a polyamide chain segment in the molecular structure of the deepening agent can form eutectic with a molecular chain segment of the nylon fiber under the condition of high-temperature baking, so that the finished nylon fabric has a washable deepening effect.
Due to the application of the technical scheme, the invention has the following advantages:
1. the invention can effectively reduce the light reflection amount of the surface of the finished chinlon fabric by introducing the fluorine-containing group into the organic silicon molecular chain segment, thereby increasing the apparent depth of the surface of the finished chinlon fabric, and reducing the cost compared with the pure fluorine-containing resin.
2. According to the invention, the polyether chain segment existing in the molecular structure of the deepening agent is utilized to improve the hydrophilic performance of the finished nylon fabric; the polysiloxane chain segment in the molecular structure of the finishing agent can also improve the hand feeling of the fabric and increase the added value of the chinlon fabric.
3. According to the molecular chain segment containing the amide group in the molecular structure of the deepening agent for the nylon fabric, which is obtained by the invention, the polyamide chain segment in the molecular structure of the deepening agent can form eutectic with the molecular chain segment of the nylon fiber under the condition of high-temperature baking according to the principle that the structure is similar to each other, so that the finished nylon fabric has a washable deepening effect.
Drawings
FIG. 1 is an infrared spectrum of a deepening agent for nylon fabric prepared in example 1;
FIG. 2 is an infrared spectrum of a deep-dyeing agent for nylon fabric prepared in example 2;
FIG. 3 is an infrared spectrum of a deep-dyeing agent for nylon fabric prepared in example 3.
Detailed Description
The technical solution of the present invention is further described with reference to the accompanying drawings and examples.
The main test indexes and the test standard method thereof in the embodiment are as follows:
apparent color depth (K/S) value: and testing the K/S values of the dyed fabric before and after finishing by using a color tester, folding the fabric to be tested into four layers, testing on the color tester, and measuring for 4 times to obtain an average value. Wherein, the larger the K/S value is, the darker the color is; the larger the L, the lighter the color, and the smaller the L, the darker the color; a indicates a range from red to green, + a indicates a shift toward red, -a indicates a shift toward green; b denotes the range from yellow to blue, + b denotes a shift toward yellow, and b denotes a shift toward blue.
Evaluation of washing resistance: referring to GB/T3921-: test 1 "test Standard.
Example 1
The embodiment provides a deepening agent for nylon fabric, and the preparation method comprises the following steps:
1. adding 100g of polyether amine ED400 and 24.3g of adipic acid into a first reaction vessel with a stirrer and a condensation reflux device, opening the condensation reflux device and the stirrer, adding 1.86g of sodium hypophosphite, starting heating, raising the temperature to 175 ℃, adding 2.48g of triphenyl phosphite, continuing heating to 220-230 ℃, and carrying out heat preservation reaction for 1-2 hours to obtain an intermediate product I.
2. 150g of octamethylcyclotetrasiloxane, 50g of trifluoropropylmethylcyclotrisiloxane and 20g of epoxy double-end cap are added into a second reaction vessel with a stirrer, the stirrer is started, the temperature is raised to 70 ℃, 0.18g of tetramethylammonium hydroxide is added, the temperature is continuously raised to 95 ℃, and after 5 hours of heat preservation reaction, an intermediate product II is obtained.
3. 200g of intermediate product II, 17.4g of intermediate product I and 93.2g of isopropanol are added into a third reaction vessel provided with a stirrer and a condensation reflux device, the stirrer and the condensation reflux device are started, the temperature is increased to 80 ℃, the isopropanol solvent is removed under reduced pressure after the reaction is carried out for 4 hours under the condition of heat preservation, and the deepening agent for the nylon fabric is obtained.
Referring to the attached figure 1, it is an infrared spectrum of the deepening agent for the nylon fabric in the embodiment, and the curve is 1647cm-1The stretching vibration peak of-CO-NH-in the secondary amide group is positioned; 1211cm-1C-F telescopic vibration absorber in fluorine-containing group introduced for organic silicon molecular chain segmentCollecting peaks; 1089cm-1Is a C-O-C stretching vibration absorption peak in a polyether chain segment; 802cm-1Is Si-C stretching vibration absorption peak; 2965. 1447cm-1Is represented by-CH3、-CH2-a stretching vibration absorption peak. These infrared characteristic peaks illustrate the synthetic deepening agent for nylon fabrics.
The obtained deepening agent for the nylon fabric is a product. The product is a light yellow viscous liquid, and is prepared into 80g/L emulsion for finishing dyed nylon fabric. The main performance indexes of the finished chinlon fabric are shown in table 1.
TABLE 1 Main Performance indices of Polyamide fabrics before and after finishing with the target products
| Fabric | K/S value | L* | a* | b* |
| Before finishing | 12.4 | 52.9 | 44.1 | 50.5 |
| After finishing | 15.9 | 50.8 | 45.7 | 52.8 |
| Washing with water for 10 times after finishing | 15.1 | 50.4 | 45.4 | 51.9 |
Example 2
1. Adding 150g of polyether amine ED400 and 70.5g of azelaic acid into a first reaction vessel with a stirrer and a condensation reflux device, opening the condensation reflux device and the stirrer, adding 4.41g of sodium hypophosphite, starting heating, raising the temperature to 175 ℃, adding 3.3g of triphenyl phosphite, continuing to raise the temperature to 220-230 ℃, and carrying out heat preservation reaction for 1-2 hours to obtain an intermediate product I.
2. 200g of octamethylcyclotetrasiloxane, 100g of trifluoropropylmethylcyclotrisiloxane and 29.8g of epoxy double-end cap are added into a second reaction vessel with a stirrer, the stirrer is started, the temperature is raised to 70 ℃, 0.34g of tetramethylammonium hydroxide is added, the temperature is continuously raised to 95 ℃, and after the heat preservation reaction is carried out for 5 hours, an intermediate product II is obtained.
3. Adding 300g of intermediate product II, 29.5g of intermediate product I and 141.2g of isopropanol into a third reaction vessel provided with a stirrer and a condensation reflux device, starting the stirrer and the condensation reflux device, heating to 80 ℃, keeping the temperature for reaction for 4 hours, and then removing the isopropanol solvent under reduced pressure to obtain the deepening agent for the nylon fabric.
Referring to the attached figure 2, it is an infrared spectrum of the deepening agent for the nylon fabric in the embodiment, and the curve is 1647cm-1The stretching vibration peak of-CO-NH-in the secondary amide group is positioned; 1208cm-1A C-F stretching vibration absorption peak in a fluorine-containing group introduced for an organic silicon molecular chain segment; 1095cm-1Is a C-O-C stretching vibration absorption peak in a polyether chain segment; 796cm-1Is Si-C stretching vibration absorption peak; 2964. 1446cm-1Is represented by-CH3、-CH2-a stretching vibration absorption peak. These infrared characteristic peaks illustrate the utility of the synthesisA deepening agent for nylon fabric.
The obtained deepening agent for the nylon fabric is a product. The product is a light yellow viscous liquid, and is prepared into 80g/L emulsion for finishing dyed nylon fabric. The main performance indexes of the finished chinlon fabric are shown in table 2.
TABLE 2 Main Performance indices of Polyamide fabrics before and after finishing with the target products
| Fabric | K/S value | L* | a* | b* |
| Before finishing | 12.4 | 52.9 | 44.1 | 50.5 |
| After finishing | 16.3 | 50.4 | 46.4 | 53.7 |
| Washing with water for 10 times after finishing | 15.6 | 50.1 | 45.8 | 53.2 |
Example 3
1. Adding 200g of polyether amine ED600 and 67.3g of sebacic acid into a first reaction vessel with a stirrer and a condensation reflux device, opening the condensation reflux device and the stirrer, adding 4g of sodium hypophosphite, starting heating, raising the temperature to 175 ℃, adding 4g of triphenyl phosphite, continuing heating to 220-230 ℃, and carrying out heat preservation reaction for 1-2 hours to obtain an intermediate product I.
2. 300g of octamethylcyclotetrasiloxane, 300g of trifluoropropylmethylcyclotrisiloxane and 59.7g of epoxy double-end cap are added into a second reaction vessel with a stirrer, the stirrer is started, the temperature is raised to 70 ℃, 0.66g of tetramethylammonium hydroxide is added, the temperature is continuously raised to 95 ℃, and after 5 hours of heat preservation reaction, an intermediate product II is obtained.
3. Adding 400g of intermediate product II, 80.2g of intermediate product I and 320g of isopropanol into a third reaction vessel provided with a stirrer and a condensation reflux device, starting the stirrer and the condensation reflux device, heating to 80 ℃, keeping the temperature for reaction for 4 hours, and then removing the isopropanol solvent under reduced pressure to obtain the deepening agent for the nylon fabric.
Referring to the attached figure 3, it is an infrared spectrogram of the deepening agent for nylon fabric provided by the embodiment, and the curve is 1646cm-1The stretching vibration peak of-CO-NH-in the secondary amide group is positioned; 1212cm-1A C-F stretching vibration absorption peak in a fluorine-containing group introduced for an organic silicon molecular chain segment; 1092cm-1Is a C-O-C stretching vibration absorption peak in a polyether chain segment; 799cm-1Is Si-C stretching vibration absorption peak; 2963. 1445cm-1Is represented by-CH3、-CH2-a stretching vibration absorption peak. These infrared characteristic peaks illustrate the synthetic deepening agent for nylon fabrics.
The obtained deepening agent for the nylon fabric is a product. The product is a light yellow viscous liquid, and is prepared into 80g/L emulsion for finishing dyed nylon fabric. The main performance indexes of the finished chinlon fabric are shown in table 3.
TABLE 3 Main Performance indices of Polyamide fabrics before and after finishing with the target products
| Fabric | K/S value | L* | a* | b* |
| Before finishing | 12.4 | 52.9 | 44.1 | 50.5 |
| After finishing | 16.1 | 53.6 | 45.9 | 51.6 |
| Washing with water for 10 times after finishing | 15.6 | 53.1 | 45.6 | 51.3 |
Claims (4)
1. A preparation method of a deepening agent for nylon fabric is characterized by comprising the following steps:
(1) adding 20 parts by mass of polyether amine and 15-20 parts by mass of organic dibasic acid into a first reaction vessel with a stirrer and a condensation reflux device, opening the condensation reflux device and the stirrer, adding sodium hypophosphite accounting for 1.5-2% of the total mass of the reaction monomers, heating to 175 ℃, adding triphenyl phosphite accounting for 1.5-2% of the total mass of the reaction monomers, continuously heating to 220-230 ℃, and carrying out heat preservation reaction for 1-2 hours to obtain an intermediate product I; the number average molecular weight of the polyether amine is 400 or 600;
(2) adding 15 parts of octamethylcyclotetrasiloxane, 5-15 parts of trifluoropropylmethylcyclotrisiloxane and 2-3 parts of epoxy double-seal head into a second reaction container with a stirrer, starting the stirrer, heating to 70-75 ℃, adding tetramethylammonium hydroxide accounting for 0.08-0.1% of the total mass of the reaction monomers, continuing heating to 90-100 ℃, and carrying out heat preservation reaction for 5-6 hours to obtain an intermediate product II;
(3) and adding 30 parts of the intermediate product II, 30-60 parts of the intermediate product I and 25-60 parts of isopropanol into a third reaction vessel provided with a stirrer and a condensation reflux device, starting the stirrer and the condensation reflux device, heating to 75-80 ℃, preserving heat, reacting for 4 hours, and then decompressing to remove the isopropanol solvent to obtain the deepening agent for the nylon fabric.
2. The preparation method of the deepening agent for the nylon fabric according to claim 1, wherein the deepening agent comprises the following steps: the organic dibasic acid is one of adipic acid, azelaic acid and sebacic acid.
3. The preparation method of the deepening agent for the nylon fabric according to claim 1, wherein the deepening agent comprises the following steps: the dosage of the isopropanol in the step (3) is 30-40% of the total mass of the intermediate product I and the intermediate product II.
4. A deep-dyeing agent for nylon fabric obtained by the preparation method of claim 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498754A (en) * | 2016-12-01 | 2017-03-15 | 南通纺织丝绸产业技术研究院 | A kind of softening agent for nylon fabric, preparation method and applications |
| CN109667155A (en) * | 2018-12-31 | 2019-04-23 | 南通纺织丝绸产业技术研究院 | It is a kind of for terylene and the organosilicon water repellent of nylon fabric, preparation method and application |
| CN110106710A (en) * | 2019-05-29 | 2019-08-09 | 苏州大学 | A kind of multifunctional fabric finishing agent and the preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106498754A (en) * | 2016-12-01 | 2017-03-15 | 南通纺织丝绸产业技术研究院 | A kind of softening agent for nylon fabric, preparation method and applications |
| CN109667155A (en) * | 2018-12-31 | 2019-04-23 | 南通纺织丝绸产业技术研究院 | It is a kind of for terylene and the organosilicon water repellent of nylon fabric, preparation method and application |
| CN110106710A (en) * | 2019-05-29 | 2019-08-09 | 苏州大学 | A kind of multifunctional fabric finishing agent and the preparation method and application thereof |
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