CN115182165A - Preparation method of denim sizing penetrating agent - Google Patents

Preparation method of denim sizing penetrating agent Download PDF

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Publication number
CN115182165A
CN115182165A CN202211027077.9A CN202211027077A CN115182165A CN 115182165 A CN115182165 A CN 115182165A CN 202211027077 A CN202211027077 A CN 202211027077A CN 115182165 A CN115182165 A CN 115182165A
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Prior art keywords
reaction kettle
preparing
sizing
denim
reaction
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CN202211027077.9A
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Chinese (zh)
Inventor
刘国义
涂胜宏
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SUZHOU LIANSHENG CHEMISTRY CO Ltd
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SUZHOU LIANSHENG CHEMISTRY CO Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32Polymers modified by chemical after-treatment
    • C08G65/321Polymers modified by chemical after-treatment with inorganic compounds
    • C08G65/327Polymers modified by chemical after-treatment with inorganic compounds containing phosphorus
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/40Reduced friction resistance, lubricant properties; Sizing compositions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to the technical field of textile dyeing and finishing, and discloses a preparation method of a jean sizing penetrant, which comprises the steps of preparing an intermediate in a reaction kettle; adding the intermediate into a reaction kettle, and stirring; adding liquid caustic soda into a reaction kettle for neutralization reaction; and adding tributyl phosphate and pure water, and fully stirring. The jean sizing penetrant prepared by the method has the advantages of good permeability, low foam, alkali resistance and environmental friendliness.

Description

Preparation method of denim sizing penetrating agent
Technical Field
The invention relates to the technical field of textile dyeing and finishing, in particular to a preparation method of a denim sizing penetrating agent.
Background
Denim is mostly a high-thick-count high-density fabric, and warp yarns of the denim need to be sized. The denim sizing aims at enhancing the friction resistance of the yarn, reducing the elongation and attaching the hairiness. Sizing yarns not only need to bear repeated friction between machines and yarns and between yarns to stop spinning, but also need to receive the test of secondary hairiness generated by the yarns in the friction process.
The sizing mechanism is as follows: after the warp yarns are sized, the sizing agent forms a layer of sizing film around the yarn body, and the sizing agent permeates into single fibers to stick the single fibers, so that the bundling property and the strength of the composite yarns are improved, and the wear-resisting strength of the yarns is enhanced. Therefore, the sizing agent has better permeability and covering property, and the good permeability of the sizing agent can improve the wear resistance of the yarn, thereby meeting the requirements of high-tension weaving, opening, beating-up and repeated stretching of the jean. The sizing agent has good covering property, can form a sizing film on the surface of the yarn to be attached to filoplume, can bear the friction of a reed and a heddle, and keeps the cloth surface smooth.
At present, the common denim sizing penetrant in the market is a compound of an anionic surfactant and a nonionic surfactant, but the existing denim sizing penetrant is not ideal in the aspects of permeability, alkali resistance, foaming property, reduction resistance and the like.
Disclosure of Invention
The invention aims to provide a preparation method of a denim sizing penetrant, and the denim sizing penetrant prepared by the method has good permeability, low foam, alkali resistance and environmental protection.
In order to achieve the aim, the invention provides a preparation method of a denim sizing penetrant, which comprises the following steps:
preparing an intermediate in a reaction kettle;
adding the intermediate into a reaction kettle, and stirring;
adding liquid alkali into the reaction kettle to perform neutralization reaction;
then tributyl phosphate and pure water are added and fully stirred.
Preferably, the preparation of the intermediate in the reaction kettle specifically comprises:
adding isomeric fatty alcohol polyoxyethylene ether (XP 30), diethylene glycol monobutyl ether and phosphorous acid into a reaction kettle in sequence;
introducing nitrogen into the reaction kettle, and stirring the materials in the reaction kettle;
heating the reaction kettle to a first set temperature;
adding phosphorus pentoxide into the reaction kettle for multiple times;
heating the reaction kettle to a second set temperature;
and adding pure water into the reaction kettle, and performing hydrolysis reaction to obtain the intermediate.
Preferably, the heterogeneous fatty alcohol polyoxyethylene ether (XP 30), diethylene glycol monobutyl ether, phosphorous acid and the phosphorus pentoxide have the following mass percentages: 77.0%, 8.0%, 1.0% and 14.0%.
Preferably, the preparation of the intermediate in the reaction kettle specifically comprises:
adding isomeric fatty alcohol-polyoxyethylene ether (JFC) and phosphorous acid into a reaction kettle in sequence;
introducing nitrogen into the reaction kettle, and stirring the materials in the reaction kettle;
heating the reaction kettle to a first set temperature;
adding phosphorus pentoxide into the reaction kettle for multiple times;
heating the reaction kettle to a second set temperature;
and adding pure water into the reaction kettle, and performing hydrolysis reaction to obtain the intermediate.
Preferably, the mass percentages of the isomeric fatty alcohol-polyoxyethylene ether, the phosphorus pentoxide and the phosphorous acid are respectively 88.0%, 10.0% and 2.0%.
Preferably, the first set temperature is 40 ℃.
Preferably, the second set temperature is 80 ℃.
Preferably, the method for preparing the denim-slash penetrant according to claim 1, wherein the hydrolysis reaction time is 1 hour.
Preferably, the reaction kettle is heated to a second set temperature, and then the method further comprises the step of carrying out an esterification reaction when the temperature of the reaction kettle is raised to 80-85 ℃, wherein the esterification reaction time is 3-4 hours.
Preferably, the adding phosphorus pentoxide into the reaction kettle for multiple times specifically comprises: the phosphorus pentoxide was added in a dispersed state 5 times over 90 min.
Therefore, compared with the denim sizing penetrant widely used in the prior art, the denim sizing penetrant prepared by the method has the advantages of better permeability, low foam, alkali resistance and environmental friendliness.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples.
Embodiment 1 of the present specification specifically discloses:
the denim sizing penetrant comprises the following components in percentage by mass:
Figure BDA0003815962000000031
the preparation method comprises the following steps:
the first step is as follows: synthesis of isomeric fatty alcohol-polyoxyethylene ether phosphate (XP 30) intermediate
Respectively weighing isomeric fatty alcohol polyoxyethylene ether (XP 30), diethylene glycol monobutyl ether and phosphorous acid in a clean reaction kettle according to mass percent, introducing nitrogen, starting a stirrer, fully stirring for 30-50 minutes, slowly heating to about 40 ℃, adding phosphorus pentoxide in a dispersing state for 5 times in 90min, slowly heating to 80 ℃, performing esterification reaction for 3-4 hours at 80-85 ℃, then adding proper pure water for hydrolysis reaction for 1 hour, cooling to below 50 ℃ after the experiment is finished, and filtering and discharging.
The second step is that: compounding of sizing penetrant
Putting the synthesized intermediate into a reaction kettle, starting stirring, slowly adding a proper amount of liquid alkali while cooling (heat release phenomenon exists due to neutralization reaction) to neutralize until the pH is =7, then adding tributyl phosphate and pure water required by the formula concentration, wherein the mass ratio of the tributyl phosphate is 3-5%, and other raw materials except the other raw materials are supplemented with the pure water. And after fully and uniformly stirring, filtering and discharging to obtain the sizing penetrant.
Embodiment 2 specifically discloses:
the denim sizing penetrant comprises the following components in percentage by mass:
88.0 percent of isomeric fatty alcohol-polyoxyethylene ether
Phosphorus pentoxide 10.0%
Phosphorous acid 2.0%
The preparation method comprises the following steps:
the first step is as follows: synthesis of isomeric fatty alcohol-polyoxyethylene ether phosphate (JFC) intermediate
Respectively weighing isomeric fatty alcohol-polyoxyethylene ether (JFC), phosphorous acid, introducing nitrogen gas, starting a stirrer, fully stirring for 30-50 minutes, slowly heating to about 40 ℃, adding phosphorus pentoxide in a dispersed state for 5 times in 90min, slowly heating to 80 ℃, carrying out esterification reaction for 3-4 hours at 80-85 ℃, then adding proper pure water for hydrolysis reaction for 1 hour, cooling to below 50 ℃ after the experiment is finished, and filtering and discharging.
The second step is that: compounding of sizing penetrant
Putting the synthesized intermediate into a reaction kettle, starting stirring, slowly adding a proper amount of liquid alkali while cooling (heat release phenomenon exists due to neutralization reaction) to neutralize until the pH is =7, then adding tributyl phosphate and pure water required by the formula concentration, wherein the mass ratio of the tributyl phosphate is 3-5%, and other raw materials except the other raw materials are supplemented with the pure water. And after fully and uniformly stirring, filtering and discharging to obtain the sizing penetrant.
The test contents, standards and methods of the denim sizing yarn penetrant prepared by the method are as follows:
solid content (non-volatile component) is prepared from ZB G73010-90
The range is as follows: 30.0. + -. 1.0% found: 30.3 percent of
Measurement of pH of aqueous surfactant solution-potentiometric method: the method is derived from the following steps of GB/T6368-93 (ISO 4316-1977) determination of pH of aqueous solution: the range is as follows: 7.0. + -. 1.0 found: 6.9
Method for testing foamability (plug measuring cylinder method) method source: GB/T13173.6-91, GB/T7462-94, and special teaching material for dyeing and finishing
Foamability (30 seconds): the range is as follows: <10.0cm found: 3.0cm
Test method for wet permeability (standard canvas settlement method): the method is from GB 5557-85
Wet penetration (unit: sec "): the range is as follows: <5.0 "found: 2.0 ″)
Alkali resistance test: the method is from HG/T4919-2016
Alkali resistance (100% NaOH, g/l) range: measured by the measurement of 120.0 g/l: 150.0g/l
Therefore, compared with the penetrant in the prior art, the penetrant for sizing denim prepared by the method has better permeability, low foam, alkali resistance and environmental protection.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the disclosed embodiments without departing from the spirit and scope of the present invention.

Claims (10)

1. The preparation method of the jean sizing penetrating agent is characterized by comprising the following steps: the method comprises the following steps:
preparing an intermediate in a reaction kettle;
adding the intermediate into a reaction kettle, and stirring;
adding liquid alkali into the reaction kettle to perform neutralization reaction;
and adding tributyl phosphate and pure water, and fully stirring.
2. The method for preparing the jean slashing penetrant according to claim 1, wherein the preparation of the intermediate in a reaction kettle specifically comprises the following steps:
adding isomeric fatty alcohol polyoxyethylene ether (XP 30), diethylene glycol monobutyl ether and phosphorous acid into a reaction kettle in sequence;
introducing nitrogen into the reaction kettle, and stirring the materials in the reaction kettle;
heating the reaction kettle to a first set temperature;
adding phosphorus pentoxide into the reaction kettle for multiple times;
heating the reaction kettle to a second set temperature;
and adding pure water into the reaction kettle, and performing hydrolysis reaction to obtain the intermediate.
3. The method for preparing the denim sizing penetrant according to claim 2, wherein the heterogeneous fatty alcohol-polyoxyethylene ether (XP 30), the diethylene glycol monobutyl ether, the phosphorous acid and the phosphorus pentoxide respectively comprise the following components in percentage by mass: 77.0%, 8.0%, 1.0% and 14.0%.
4. The method for preparing the jean slashing penetrant according to claim 1, wherein the preparation of the intermediate in a reaction kettle specifically comprises the following steps:
adding isomeric fatty alcohol-polyoxyethylene ether (JFC) and phosphorous acid into a reaction kettle in sequence;
introducing nitrogen into the reaction kettle, and stirring the materials in the reaction kettle;
heating the reaction kettle to a first set temperature;
adding phosphorus pentoxide into the reaction kettle for multiple times;
heating the reaction kettle to a second set temperature;
and adding pure water into the reaction kettle, and performing hydrolysis reaction to obtain the intermediate.
5. The method for preparing the denim sizing penetrant according to claim 4, wherein the mass percentages of the isomeric fatty alcohol-polyoxyethylene ether, the phosphorus pentoxide and the phosphorous acid are 88.0%, 10.0% and 2.0%, respectively.
6. The method for preparing a denim slashing penetrant according to claim 2 or 4, wherein the first set temperature is 40 ℃.
7. The method for preparing a denim slash penetrant according to claim 2 or 4, wherein the second set temperature is 80 ℃.
8. The method for preparing the denim sizing penetrant according to claim 2 or 4, the method for preparing the denim sizing penetrant according to claim 1, and the time of the hydrolysis reaction is 1 hour.
9. The method for preparing the denim-slash penetrant according to claim 2 or 4, wherein the reaction kettle is heated to a second set temperature, and then the method further comprises performing an esterification reaction when the temperature of the reaction kettle is raised to 80-85 ℃, wherein the esterification reaction time is 3-4 hours.
10. The method for preparing the denim sizing penetrant according to claim 2 or 4, wherein the adding phosphorus pentoxide into the reaction kettle in multiple times specifically comprises: the phosphorus pentoxide was added in a dispersed state 5 times over 90 min.
CN202211027077.9A 2022-08-25 2022-08-25 Preparation method of denim sizing penetrating agent Pending CN115182165A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575804A (en) * 2009-04-25 2009-11-11 中山市巴斯基化工有限公司 Alkali-resistant penetrant for short-process pretreatment of pure-cotton woven fabric
CN102797149A (en) * 2012-07-30 2012-11-28 浙江安诺其助剂有限公司 Alkali-resistant refined penetrant and preparation method thereof
CN106120319A (en) * 2016-07-01 2016-11-16 潘明华 A kind of silkete penetrating agent and preparation method thereof
CN108130758A (en) * 2017-12-26 2018-06-08 广东奥克化学有限公司 A kind of bleeding agent and preparation method thereof
CN108611850A (en) * 2018-06-22 2018-10-02 淄博鲁瑞精细化工有限公司 The preparation method of the low bubble concise bleeding agent of phosphate
CN110820378A (en) * 2019-09-11 2020-02-21 宜兴市中达化工有限公司 Production method of air exhaust agent for denim dyeing and cheese dyeing

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575804A (en) * 2009-04-25 2009-11-11 中山市巴斯基化工有限公司 Alkali-resistant penetrant for short-process pretreatment of pure-cotton woven fabric
CN102797149A (en) * 2012-07-30 2012-11-28 浙江安诺其助剂有限公司 Alkali-resistant refined penetrant and preparation method thereof
CN106120319A (en) * 2016-07-01 2016-11-16 潘明华 A kind of silkete penetrating agent and preparation method thereof
CN108130758A (en) * 2017-12-26 2018-06-08 广东奥克化学有限公司 A kind of bleeding agent and preparation method thereof
CN108611850A (en) * 2018-06-22 2018-10-02 淄博鲁瑞精细化工有限公司 The preparation method of the low bubble concise bleeding agent of phosphate
CN110820378A (en) * 2019-09-11 2020-02-21 宜兴市中达化工有限公司 Production method of air exhaust agent for denim dyeing and cheese dyeing

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