CN111188211A - Preparation method of stain-proofing agent for washing jeans wear - Google Patents
Preparation method of stain-proofing agent for washing jeans wear Download PDFInfo
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- CN111188211A CN111188211A CN201911153860.8A CN201911153860A CN111188211A CN 111188211 A CN111188211 A CN 111188211A CN 201911153860 A CN201911153860 A CN 201911153860A CN 111188211 A CN111188211 A CN 111188211A
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- dye
- washing
- jeans wear
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- preset temperature
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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
- D06P5/12—Reserving parts of the material before dyeing or printing ; Locally decreasing dye affinity by chemical means
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
- D06L1/12—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polyesters Or Polycarbonates (AREA)
- Detergent Compositions (AREA)
Abstract
The invention provides a preparation method of a dye-resistant agent for washing jeans wear, which comprises the following steps of adding a mixture of terephthalic acid and phthalic acid and ethylene glycol into a container, adding a catalyst into the container to form a mixture, introducing inert gas into the container for protection, heating the mixture to a first preset temperature for esterification reaction, heating to a second preset temperature after the reaction is finished, carrying out pre-polycondensation, adding polyoxyethylene ether under the protection of the inert gas, vacuumizing, heating to a third preset temperature for polycondensation reaction, and obtaining the dye-resistant agent for washing jeans wear.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of dye-proofing agents, in particular to a preparation method of a dye-proofing agent for washing jeans wear.
[ background of the invention ]
With the increasingly fierce market competition, the costs of raw materials, labor, factory buildings and the like are greatly increased, and the traditional method for manufacturing the denim by using cotton fibers is slowly changed into the method for manufacturing the denim by using polyester-cotton blended yarns or polyester-cotton-spandex blended yarns. The conversion of raw materials brings more and more style changes to jeans, but some problems in the manufacturing process of the jeans also follow. Because the dye-resist can not completely solve the problem that indigo dye is re-dyed on polyester-cotton blended jeans, a good-effect dye-resist for washing polyester-cotton jeans garments is urgently needed in the market at present.
In view of the above, there is a need to provide a novel method for preparing a dye-resist for washing jeans garments to overcome the above-mentioned drawbacks.
[ summary of the invention ]
The invention aims to provide a preparation method of a dye-resistant agent for washing jeans wear, the dye-resistant agent prepared by the invention has good affinity with polyester-cotton fabrics, and can effectively prevent indigo dye from being stained on the polyester-cotton blended fabrics.
In order to achieve the above object, the present invention provides a method for preparing a stain-proofing agent for washing jeans wear, comprising the steps of,
adding a mixture of terephthalic acid and phthalic acid and ethylene glycol into a container, adding a catalyst into the container to form a mixture, introducing inert gas into the container for protection, heating the mixture to a first preset temperature for esterification reaction, heating to a second preset temperature after the reaction is finished, carrying out pre-polycondensation, adding polyoxyethylene ether under the protection of the inert gas, vacuumizing, heating to a third preset temperature for polycondensation reaction, and obtaining the dye-resistant agent for washing the jeans wear.
Specifically, the mass content of terephthalic acid in the mixture of terephthalic acid and phthalic acid is 0-90%, the mass content of phthalic acid is 0-90%, and the number average molecular weight of polyoxyethylene ether is 100-50000.
Specifically, the container is a four-neck flask, and the inert gas is nitrogen.
Specifically, the viscosity of the pre-polycondensation reaction is 0.1-0.15 deciliter per gram.
Specifically, the temperature range of the first preset temperature is as follows: 180-200 ℃, wherein the second preset temperature range is as follows: 220-240 ℃, wherein the pre-polycondensation time is as follows: 1-2 hours, wherein the third preset temperature range is as follows: 260-290 ℃.
Specifically, the catalyst accounts for 0.1-0.3% of the mass of the mixture of phthalic acid and phthalic acid, and is titanium dioxide.
Specifically, the pressure of the polycondensation reaction is 200-300 pa, the average molecular weight of the dye-resist agent for washing the jeans wear is 2000-100000, and the intrinsic viscosity of the dye-resist agent for washing the jeans wear is more than 0.39 deciliter/gram.
Compared with the prior art, the preparation method of the denim washing resist agent has the advantages that the denim washing resist agent prepared by the preparation method is prepared by taking terephthalic acid, phthalic acid and ethylene glycol as raw materials through an esterification reaction under the action of a catalyst, the denim washing resist agent has good affinity with polyester-cotton fabrics, and indigo dye can be effectively prevented from being stained on the polyester-cotton blended fabrics.
[ detailed description ] embodiments
In order to make the objects, technical solutions and advantageous effects of the present invention more apparent, the present invention is further described in detail with reference to the following detailed description. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides a preparation method of a dye-resistant agent for washing jeans wear, which comprises the following steps:
adding a mixture of terephthalic acid and phthalic acid and ethylene glycol into a container, adding a catalyst into the container to form a mixture, introducing inert gas into the container for protection, heating the mixture to a first preset temperature for esterification reaction, heating to a second preset temperature after the reaction is finished, carrying out pre-polycondensation, adding polyoxyethylene ether under the protection of the inert gas, vacuumizing, heating to a third preset temperature for polycondensation reaction, and obtaining the dye-resistant agent for washing the jeans wear.
Specifically, the mass content of terephthalic acid in the mixture of terephthalic acid and phthalic acid is 0-90%, the mass content of phthalic acid is 0-90%, and the number average molecular weight of polyoxyethylene ether is 100-50000.
Specifically, the container is a four-neck flask, and the inert gas is nitrogen.
Specifically, the viscosity of the pre-polycondensation reaction is 0.1-0.15 deciliter/gram.
Specifically, the temperature range of the first preset temperature is as follows: 180-200 ℃, wherein the second preset temperature range is as follows: 220-240 ℃, wherein the pre-polycondensation time is as follows: 1-2 hours, wherein the third preset temperature range is as follows: 260-290 ℃.
Specifically, the catalyst accounts for 0.1-0.3% of the mass of the mixture of phthalic acid and phthalic acid, and is titanium dioxide.
Specifically, the pressure of the polycondensation reaction is 200-300 pa, the average molecular weight of the dye-resist agent for washing the jeans wear is 2000-100000, and the intrinsic viscosity of the dye-resist agent for washing the jeans wear is more than 0.39 deciliter/gram.
Example 1
Adding a mixture formed by mixing 166.13 g of terephthalic acid and 332.26 g of phthalic acid and 186.00 g of ethylene glycol into a four-neck flask, adding 1.36 g of titanium dioxide, introducing nitrogen into the four-neck flask for protection, heating to 200 ℃ for esterification, finishing the reaction when the generated water content is 54.00 g, heating to 240 ℃ for pre-polycondensation for 1.5 hours, wherein the viscosity of the reaction during pre-polycondensation reaches 0.13 dl/g, adding 3.45 kg of polyoxyethylene ether with the number-average molecular weight of 1200 under the protection of nitrogen, vacuumizing, heating to 290 ℃ for polycondensation, and obtaining the water-washing dye resist A for jeans wear.
Example 2
Adding a mixture formed by mixing 332.26 g of terephthalic acid and 332.26 g of phthalic acid and 206.00 g of ethylene glycol into a four-neck flask, adding 1.96 g of titanium dioxide, introducing nitrogen into the four-neck flask for protection, heating to 200 ℃ for esterification, finishing the reaction when the generated water content is 72.00 g, heating to 240 ℃ for pre-polycondensation for 1.9 hours, wherein the viscosity of the reaction during pre-polycondensation reaches 0.15 deciliter/g, adding 4.23 kg of polyoxyethylene ether with the number-average molecular weight of 2200 under the protection of nitrogen, vacuumizing, heating to 290 ℃ for polycondensation, and obtaining the dye-resistant agent B for washing jeans wear.
Example 3
332.26 g of terephthalic acid and 166.13 g of phthalic acid are mixed to form a mixture, the mixture and 176.00 g of ethylene glycol are added into a four-neck flask, 1.49 g of titanium dioxide are added, nitrogen is introduced into the four-neck flask for protection, the temperature is raised to 200 ℃ for esterification, when the generated water content is 54.00 g, the reaction is ended, the temperature is raised to 240 ℃ for pre-polycondensation for 1.6 hours, the viscosity of the reaction during pre-polycondensation reaches 0.14 dl/g, 4.89 kg of polyoxyethylene ether with the number-average molecular weight of 3200 is added under the protection of nitrogen, the mixture is vacuumized, the temperature is raised to 290 ℃ for polycondensation, and the dye-resistant agent C for washing jeans garments is obtained.
Example 4
Adding a mixture formed by mixing 332.26 g of terephthalic acid and 166.13 g of phthalic acid and 176.00 g of ethylene glycol into a four-neck flask, adding 1.32 g of titanium dioxide, introducing nitrogen into the four-neck flask for protection, heating to 200 ℃ for esterification, finishing the reaction when the generated water content is 54.00 g, heating to 240 ℃ for pre-polycondensation for 1.6 hours, wherein the viscosity of the reaction during pre-polycondensation reaches 0.13 dl/g, adding 2.98 kg of polyoxyethylene ether with the number-average molecular weight of 1200 under the protection of nitrogen, vacuumizing, heating to 290 ℃ for polycondensation, and obtaining the dye-resistant agent D for washing jeans wear.
Example 5
Adding a mixture formed by mixing 332.26 g of terephthalic acid and 166.13 g of phthalic acid and 189.00 g of ethylene glycol into a four-neck flask, adding 1.32 g of titanium dioxide, introducing nitrogen into the four-neck flask for protection, heating to 200 ℃ for esterification, finishing the reaction when the generated water content is 54.00 g, heating to 240 ℃ for pre-polycondensation for 1.7 hours, wherein the viscosity of the reaction during pre-polycondensation reaches 0.15 deciliter/g, adding 2.98 kg of polyoxyethylene ether with the number-average molecular weight of 8000 under the protection of nitrogen, vacuumizing, heating to 290 ℃ for polycondensation, and obtaining the dye-resistant agent E for washing jeans garments.
Test examples
The dye-proofing agents A to E obtained in the embodiment 1 to 5 and common dye-proofing agents are respectively subjected to dye-proofing effect tests, the pattern formation effect of the jeans trouser legs is respectively subjected to sensory evaluation, the dyeing effect is divided into a full point of 5 and is graded within the range of 0 to 5, meanwhile, the whiteness of the pure cotton/polyester cotton white cloth subjected to washing is tested, and the test process and the test results are shown in the following table 1,
equipment: a washing test machine; material distribution: 3 twill polyester cotton blended jeans legs, 1 piece of 10cm by 10cm white polyester cotton blended fabric and 1 piece of 10cm by 10cm white pure cotton fabric; raw materials: 5 g of neutral cellulase, 15 g of buffer agent and 8 kg of water; washing process conditions are as follows: 55 ℃ for 60 ℃ and pH 6.5.
Table 1:
in example 4, 332.26 g of terephthalic acid, 166.13 g of phthalic acid, 176.00 g of ethylene glycol and 1.32 g of titanium dioxide are taken to be subjected to precondensation for 1.6 hours, the viscosity of the reaction during the precondensation reaches 0.13 dl/g, 2.98 kg of polyoxyethylene ether with the number average molecular weight of 1200 is added, and the values of the whiteness of the pure cotton white cloth and the whiteness of the polyester cotton white cloth of the stain-resistant agent in example 4 under the same washing water process conditions are the highest.
As can be seen from table 1, the whiteness values of the pure cotton white cloth and the whiteness values of the polyester cotton white cloth of the stain-proofing agent prepared in the examples 1 to 5 of the present invention are higher than the whiteness values of the pure cotton white cloth and the whiteness values of the polyester cotton white cloth of the common stain-proofing agent and the stain-proofing agent-free agent under the same washing process conditions, so that the stain-proofing effect of the stain-proofing agent prepared in the examples 1 to 5 of the present invention is better; the dye-resistant agent prepared by the invention has good affinity with the polyester-cotton fabric, and can effectively prevent indigo dye from being stained on the polyester-cotton blended fabric.
The invention is not limited solely to that described in the specification and embodiments, and additional advantages and modifications will readily occur to those skilled in the art, so that the invention is not limited to the specific details, representative apparatus, and examples shown and described herein, without departing from the spirit and scope of the general concept as defined by the appended claims and their equivalents.
Claims (7)
1. A preparation method of a dye-resistant agent for washing jeans wear is characterized by comprising the following steps,
adding a mixture of terephthalic acid and phthalic acid and ethylene glycol into a container, adding a catalyst into the container to form a mixture, introducing inert gas into the container for protection, heating the mixture to a first preset temperature for esterification reaction, heating to a second preset temperature after the reaction is finished, carrying out pre-polycondensation, adding polyoxyethylene ether under the protection of the inert gas, vacuumizing, heating to a third preset temperature for polycondensation reaction, and obtaining the dye-resistant agent for washing the jeans wear.
2. The method for preparing the dye-proofing agent for washing jeans wear according to claim 1, wherein the mixture of terephthalic acid and phthalic acid contains 0-90% by mass of terephthalic acid, 0-90% by mass of phthalic acid, and the polyoxyethylene ether has a number average molecular weight of 100-50000.
3. The method for preparing a dye resist for washing jeans wear according to claim 1, wherein the container is a four-neck flask, and the inert gas is nitrogen.
4. The method for preparing the dye resist for washing jeans wear according to claim 1, wherein the viscosity of the pre-polycondensation reaction is 0.1 to 0.15 dl/g.
5. The method for preparing a dye resist for washing jeans wear according to claim 1, wherein the temperature range of the first preset temperature is as follows: 180-200 ℃, wherein the second preset temperature range is as follows: 220-240 ℃, wherein the pre-polycondensation time is as follows: 1-2 hours, wherein the third preset temperature range is as follows: 260-290 ℃.
6. The method for preparing the dye-proofing agent for washing jeans wear according to claim 1, wherein the catalyst accounts for 0.1-0.3% of the mass of the mixture of phthalic acid and phthalic acid, and the catalyst is titanium dioxide.
7. The method for preparing the water-washable dye-resist for jeans wear according to claim 1, wherein the pressure of the polycondensation reaction is 200-300 pa, the average molecular weight of the water-washable dye-resist for jeans wear is 2000-100000, and the intrinsic viscosity of the water-washable dye-resist for jeans wear is greater than 0.39 dl/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911153860.8A CN111188211A (en) | 2019-11-22 | 2019-11-22 | Preparation method of stain-proofing agent for washing jeans wear |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911153860.8A CN111188211A (en) | 2019-11-22 | 2019-11-22 | Preparation method of stain-proofing agent for washing jeans wear |
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| CN111188211A true CN111188211A (en) | 2020-05-22 |
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| CN201911153860.8A Pending CN111188211A (en) | 2019-11-22 | 2019-11-22 | Preparation method of stain-proofing agent for washing jeans wear |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114016293A (en) * | 2021-12-15 | 2022-02-08 | 张家港市德宝化工有限公司 | Anti-reverse staining agent for jeans and preparation method thereof |
| CN117051610A (en) * | 2023-09-06 | 2023-11-14 | 韶关市北纺智造科技有限公司 | Washing water dyeing resist for jean elastic fabric and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3736294A (en) * | 1967-01-24 | 1973-05-29 | Asahi Chemical Ind | Poly(ethylene terephthalate) from bis(hydroxyethyl)terephthalate and terephthalic acid |
| CN102493234A (en) * | 2011-12-22 | 2012-06-13 | 东莞市广利行洗涤原料有限公司 | Reserving agent for washing jean garments and preparation method thereof |
| CN109267405A (en) * | 2018-08-02 | 2019-01-25 | 广州大久生物科技有限公司 | Resist printing stabilizing additive composition and its preparation method and application and compounding cellulase and its application |
-
2019
- 2019-11-22 CN CN201911153860.8A patent/CN111188211A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3736294A (en) * | 1967-01-24 | 1973-05-29 | Asahi Chemical Ind | Poly(ethylene terephthalate) from bis(hydroxyethyl)terephthalate and terephthalic acid |
| CN102493234A (en) * | 2011-12-22 | 2012-06-13 | 东莞市广利行洗涤原料有限公司 | Reserving agent for washing jean garments and preparation method thereof |
| CN109267405A (en) * | 2018-08-02 | 2019-01-25 | 广州大久生物科技有限公司 | Resist printing stabilizing additive composition and its preparation method and application and compounding cellulase and its application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114016293A (en) * | 2021-12-15 | 2022-02-08 | 张家港市德宝化工有限公司 | Anti-reverse staining agent for jeans and preparation method thereof |
| CN117051610A (en) * | 2023-09-06 | 2023-11-14 | 韶关市北纺智造科技有限公司 | Washing water dyeing resist for jean elastic fabric and preparation method thereof |
| CN117051610B (en) * | 2023-09-06 | 2024-02-23 | 韶关市北纺智造科技有限公司 | Washing water dyeing resist for jean elastic fabric and preparation method thereof |
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Application publication date: 20200522 |
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