CN114000355A - Hydrophilic elastic silicone oil finishing agent for pure cotton fabric and preparation method thereof - Google Patents

Hydrophilic elastic silicone oil finishing agent for pure cotton fabric and preparation method thereof Download PDF

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Publication number
CN114000355A
CN114000355A CN202111318498.2A CN202111318498A CN114000355A CN 114000355 A CN114000355 A CN 114000355A CN 202111318498 A CN202111318498 A CN 202111318498A CN 114000355 A CN114000355 A CN 114000355A
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silicone oil
finishing agent
hydrophilic
pure cotton
cotton fabric
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李兵
涂胜宏
谭函彬
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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
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/647Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
    • 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
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42Block-or graft-polymers containing polysiloxane sequences
    • C08G77/46Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
    • 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
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • 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
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
    • 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
    • D06M2200/50Modified hand or grip properties; Softening compositions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (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 discloses a hydrophilic, smooth and elastic silicone oil finishing agent for pure cotton fabric and a preparation method thereof, wherein the finishing agent comprises the following components in percentage by weight: high molecular weight Polymer: 30-40%, organic acid: 0.1% -0.5% deionized water: 50% -80%; the high molecular polymer is poly quaternary ammonium polyether polysiloxane. According to the hydrophilic smooth and elastic silicone oil finishing agent for the pure cotton fabric and the preparation method thereof, the prepared finishing agent has good hydrophilicity, strong hygroscopicity, good washability and no phenol yellowing on cotton fibers, can endow the pure cotton fabric with an excellent smooth and elastic style, improves the stiffness of the fabric, and is natural and free of greasy skin-friendly hand feeling.

Description

Hydrophilic elastic silicone oil finishing agent for pure cotton fabric and preparation method thereof
Technical Field
The invention relates to the technical field of dyeing and finishing processing, in particular to a hydrophilic and elastic silicone oil finishing agent for pure cotton fabric and a preparation method thereof.
Background
The combed cotton is woven by the best long-staple cotton and a special process, the fabric texture is finer, smoother, more elastic, higher in quality, more prominent in air permeability and water absorbability than that of common pure cotton, and the quality level of texture, washing fastness and durability of the combed cotton is superior to that of common pure cotton. The mercerized cotton belongs to the best product of cotton materials in the eyes of the pedestrians, and not only has the characteristics of the original cotton, but also has the luster and soft hand feeling of silk. Combed cotton and mercerized cotton become one of the main fabrics of modern clothes, and are popular with people, and the combed cotton and the mercerized cotton are both obtained by treating pure cotton fabrics with a finishing agent.
The existing hydrophilic smooth and elastic finishing agent for the pure cotton fabric has the following problems: 1. the conventional silicone oil can provide various styles, but has no hydrophilicity, so that the wearing comfort of the clothes is reduced; 2. the common hydrophilic silicone oil has single hand feeling and style, and can not meet the style requirements of various high-end fabrics on the market; 3. generally, silicone oil has yellowing and phenol has yellowing.
Disclosure of Invention
The invention aims to provide a hydrophilic smooth and elastic silicone oil finishing agent for pure cotton fabric and a preparation method thereof.
In order to achieve the purpose, the invention provides a hydrophilic elastic silicone oil finishing agent for pure cotton fabric, which comprises the following components in percentage by weight:
high molecular weight Polymer: 30 to 40 percent
Organic acid: 0.1 to 0.5 percent
Deionized water: 50% -80%;
the high molecular polymer is poly quaternary ammonium polyether polysiloxane, and the structural general formula is as follows:
Figure BDA0003344623400000021
wherein A is-Is Cl-、Br-、I-、CH3COO-、C3H7COO-One or more of laurate, etc.; c is 0-35, d is 0-40, n is 200-1000, and m is 2-100;
when m is more than or equal to 100 and less than or equal to 1000, the silicone oil finishing agent can enable the cotton material to have certain softness and good sliding and elastic effects, and when c is 5-10, d is more than or equal to 10-100, the silicone oil finishing agent can enable the cotton material to have good hydrophilicity;
non-primary amino (-NH)2) Secondary amine (-NRH), little or no tertiary amine (-NR)1R2) After high-temperature shaping (the temperature is higher than 180-200 ℃), the hydrophilicity of the polyether is not reduced and is durable.
Preferably, the poly quaternary ammonium polyether polysiloxane is prepared by adding allyl epoxy polyether and hydrogen-terminated silicone oil and then reacting with tetramethyl hexamethylene diamine salt.
Preferably, the molecular weight of the terminal hydrogen silicone oil is between 10000-30000; the allyl epoxy polyether has a molecular weight of between 1000-3000.
A preparation method of a hydrophilic, smooth and elastic silicone oil finishing agent for pure cotton fabric is characterized by comprising the following steps:
(1) adding the hydrogen-terminated silicone oil, the allyl epoxy polyether mixture and an organic solvent into a reactor, heating, adding a catalyst in batches at the temperature of 45-85 ℃, and reacting for 4-12 hours at the temperature of 50-100 ℃ to obtain an intermediate product, namely epoxy polyether-terminated silicone oil;
the reaction equation is as follows:
Figure BDA0003344623400000031
(2) adding the epoxy-terminated polyether silicone oil obtained in the step (1) into a mixture of the acidified tetramethylhexamethylenediamine salt and the organic solvent, heating to 60-120 ℃, reacting for 12-60 hours, and then cooling to 50 ℃ to obtain a product, namely the poly-quaternary ammonium polyether polysiloxane;
the reaction equation is as follows:
Figure BDA0003344623400000032
(3) and (3) slowly adding part of water into the poly-quaternary ammonium polyether polysiloxane obtained in the step (2) for dilution, stirring for a period of time, slowly adding an organic acid to adjust the pH value to 4.5-6.5, slowly adding the rest deionized water in several times, filtering and discharging to obtain the target product.
Preferably, the organic solvent is one or more of diethylene glycol butyl ether, propylene glycol, N, N-dimethylformamide, ethylene glycol monobutyl ether, ethyl acetate, isopropanol and the like.
Preferably, the catalyst in the step (1) is a platinum catalyst, the weight percentage of the catalyst is 0.05% -0.1%, and the molar ratio of the hydrogen-terminated silicone oil to the allyl epoxy polyether is 1: 1-1.2.
Preferably, the weight percentage of the organic solvent in the step (2) is 40-70%, and the weight ratio of the epoxy polyether silicone oil to the tetramethylhexamethylene diamine salt is 100: 1-500: 1.
Preferably, the structure of the tetramethylhexamethylenediamine salt in the step (2) is as follows:
Figure BDA0003344623400000041
wherein A is-Is Cl-、Br-、I-、CH3COO-、C3H7COO-One of laurate radical and the like.
Preferably, in the step (3), the weight percentage of the poly-quaternary ammonium polyether polysiloxane is 30-40%; the weight percentage of the organic acid is 0.1 to 0.5 percent; the weight percentage of the water is 68.9-45.5%.
Preferably, in the step (3), the organic acid is added after being uniformly mixed with part of water before being added; the organic acid is one or more of formic acid, glacial acetic acid and citric acid.
The invention has the beneficial effects that:
1) on a high-molecular-weight silane chain, polyether with large molecular weight is introduced to endow the fabric with excellent hydrophilicity;
2) then, salifying with tetramethylhexamethylenediamine quaternary ammonium to form quaternary ammonium polysiloxane, wherein the cationic silicone oil is combined with the anion on the fabric by radical and ionic bond, so that the washability and the hand feeling are improved;
3) quaternary ammonium siloxane yellowness becomes low;
4) the polysiloxane with large molecular weight can form a film on the surface of the fabric, and can endow the fabric with smooth, soft and elastic handfeel.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The present invention will be further described with reference to examples, in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
The following raw materials were provided in the following metered weights: 22.5 parts by mass of hydrogen-terminated silicone oil with the molecular weight of 15000, 4.5 parts by mass of allyl epoxy polyether with the molecular weight of 1500, 1% of platinum catalyst: 0.27 part by mass, tetramethylhexamethylenediamine: 1.0 part by mass, lauric acid: 2.0 parts by mass of ethylene glycol monobutyl ether: 15 parts by mass, acetic acid: 0.3 part by mass and 54.43 parts by mass of deionized water.
The preparation process comprises the following steps:
1) adding hydrogen silicone oil and allyl epoxy polyether into a reactor, heating to 50 ℃, dropwise adding 1% platinum catalyst, and reacting for 6 hours at 95 ℃;
2) adding tetramethylhexamethylenediamine and ethylene glycol monobutyl ether which are acidized by lauric acid into the reaction, heating to 78 ℃, reacting for 16 hours, and cooling to 50 ℃;
3) slowly adding 10 parts by mass of water, stirring for 10 minutes, uniformly mixing acetic acid and 10 parts by mass of water, and slowly adding; ) And slowly adding the rest deionized water in several times, filtering and discharging to obtain the hydrophilic smooth elastic silicone oil finishing agent for cotton.
Example 2
The following raw materials were provided in the following metered weights: 24.0 parts by mass of hydrogen-terminated silicone oil with molecular weight of 20000, 7.0 parts by mass of allyl epoxy polyether with molecular weight of 2500, 1% of platinum catalyst: 0.3 part by mass, tetramethylhexamethylenediamine: 2.0 parts by mass, 36.5% hydrochloric acid: 2.0 parts by mass, ethyl acetate: 13 parts by mass, acetic acid: 0.3 part by mass and 51.4 parts by mass of deionized water.
The preparation process comprises the following steps:
1) adding hydrogen silicone oil and allyl epoxy polyether into a reactor, heating to 50 ℃, dropwise adding one percent of platinum catalyst, and reacting for 6 hours at 100 ℃;
2) adding hydrochloric acid acidified tetramethyl hexanediamine and ethyl acetate into the reaction, heating to 90 ℃, reacting for 12 hours, and cooling to 50 ℃;
3) slowly adding 10 parts by mass of water, stirring for 10 minutes, uniformly mixing acetic acid and 10 parts by mass of water, and slowly adding; and slowly adding the rest deionized water in several times, filtering and discharging to obtain the hydrophilic smooth elastic silicone oil finishing agent for cotton.
Example 3
The following raw materials were provided in the following metered weights: 24.0 parts by mass of hydrogen-terminated silicone oil with the molecular weight of 18000, 6.0 parts by mass of allyl epoxy polyether with the molecular weight of 2000, 1% of platinum catalyst: 0.3 part by mass, tetramethylhexamethylenediamine: 1.5 parts by mass, glacial acetic acid: 1.0 part by mass, diethylene glycol monobutyl ether: 15 parts by mass, acetic acid: 0.3 part by mass and 51.9 parts by mass of deionized water.
The preparation process comprises the following steps:
1) adding hydrogen silicone oil and allyl epoxy polyether into a reactor, heating to 50 ℃, dropwise adding one percent of platinum catalyst, and reacting for 6 hours at 95 ℃;
2) adding tetramethylhexanediamine and diethylene glycol monobutyl ether which are acidized by lauric acid into the reaction, heating to 105 ℃, reacting for 8 hours, and cooling to 50 ℃;
3) slowly adding 10 parts by mass of water, stirring for 10 minutes, uniformly mixing acetic acid and 10 parts by mass of water, and slowly adding; and slowly adding the rest deionized water in several times, filtering and discharging to obtain the hydrophilic smooth elastic silicone oil finishing agent for cotton.
The hydrophilic silicone oil finishing agent for cotton prepared in each example was subjected to hand feeling, whiteness, hydrophilicity, and washability tests, respectively, using commercially available hydrophilic silicone oil for pure cotton as a comparative example. The following is a demonstration of the specific experimental process and the data obtained.
(I) hand feeling, whiteness, hydrophilicity experiments
Taking white combed cotton as an experimental object, the solid content of the emulsion product is 15%, the dosage is 100g/L, and the emulsion product is soaked and rolled → dried (100 ℃) → shaping (160 ℃, 30 seconds) → moisture regain for 4 hours. The hydrophilicity (measured according to HG/T4917-2016 method), whiteness, and comparative hand feel were measured. The results are shown in the following table.
Figure BDA0003344623400000061
Note: the hand was best at 5 points and worst at 1.
In conclusion, the hydrophilic, smooth and elastic silicon oil finishing agent for cotton, prepared by the invention, can endow pure cotton fabric with smooth and elastic hand feeling, natural and non-greasy skin-friendly hand feeling, and has the characteristics of strong hygroscopicity and low yellowing.
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 invention without departing from the spirit and scope of the invention.

Claims (10)

1. The hydrophilic elastic silicone oil finishing agent for the pure cotton fabric is characterized in that: comprises the following components in percentage by weight:
high molecular weight Polymer: 30 to 40 percent
Organic acid: 0.1 to 0.5 percent
Deionized water: 50% -80%;
the high molecular polymer is poly quaternary ammonium polyether polysiloxane, and the structural general formula is as follows:
Figure FDA0003344623390000011
wherein A is-Is Cl-、Br-、I-、CH3COO-、C3H7COO-One or more of laurate, etc.; c is 0 to 35, d is 0 to 40, n is 200 to 1000, and m is 2 to 100.
2. The hydrophilic slippery elastic silicone oil finishing agent for the pure cotton fabric as claimed in claim 1, which is characterized in that: the poly quaternary ammonium base polyether polysiloxane is prepared by adding allyl epoxy polyether and hydrogen-terminated silicone oil and then reacting with tetramethyl hexamethylene diamine salt.
3. The hydrophilic slippery elastic silicone oil finishing agent for the pure cotton fabric as claimed in claim 2, which is characterized in that: the molecular weight of the hydrogen-terminated silicone oil is 10000-30000; the allyl epoxy polyether has a molecular weight of between 1000-3000.
4. A method for preparing the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric according to claims 1 to 3, which is characterized by comprising the following steps:
(1) adding the hydrogen-terminated silicone oil, the allyl epoxy polyether mixture and an organic solvent into a reactor, heating, adding a catalyst in batches at the temperature of 45-85 ℃, and reacting for 4-12 hours at the temperature of 50-100 ℃ to obtain an intermediate product, namely epoxy polyether-terminated silicone oil;
the reaction equation is as follows:
Figure FDA0003344623390000021
(2) adding the epoxy-terminated polyether silicone oil obtained in the step (1) into a mixture of the acidified tetramethylhexamethylenediamine salt and the organic solvent, heating to 60-120 ℃, reacting for 12-60 hours, and then cooling to 50 ℃ to obtain a product, namely the poly-quaternary ammonium polyether polysiloxane;
the reaction equation is as follows:
Figure FDA0003344623390000022
(3) and (3) slowly adding part of water into the poly-quaternary ammonium polyether polysiloxane obtained in the step (2) for dilution, stirring for a period of time, slowly adding an organic acid to adjust the pH value to 4.5-6.5, slowly adding the rest deionized water in several times, filtering and discharging to obtain the target product.
5. The preparation method of the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric, according to claim 4, is characterized in that: the organic solvent is one or more of diethylene glycol butyl ether, propylene glycol, N, N-dimethylformamide, ethylene glycol monobutyl ether, ethyl acetate, isopropanol and the like.
6. The preparation method of the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric, according to claim 4, is characterized in that: the catalyst in the step (1) is a platinum catalyst, the weight percentage of the catalyst is 0.05-0.1%, and the molar ratio of the hydrogen-terminated silicone oil to the allyl epoxy polyether is 1: 1-1.2.
7. The preparation method of the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric, according to claim 4, is characterized in that: the weight percentage of the organic solvent in the step (2) is 40-70%, and the weight ratio of the epoxy polyether silicone oil to the tetramethylhexamethylene diamine salt is 100: 1-500: 1.
8. The preparation method of the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric, according to claim 4, is characterized in that: the structure of the tetramethylhexamethylenediamine salt in the step (2) is as follows:
Figure FDA0003344623390000031
wherein A is-Is Cl-、Br-、I-、CH3COO-、C3H7COO-One of laurate radical and the like.
9. The preparation method of the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric, according to claim 4, is characterized in that: in the step (3), the weight percentage of the poly quaternary ammonium polyether polysiloxane is 30-40%; the weight percentage of the organic acid is 0.1 to 0.5 percent; the weight percentage of the water is 68.9-45.5%.
10. The preparation method of the hydrophilic and elastic silicone oil finishing agent for the pure cotton fabric, according to claim 4, is characterized in that: in the step (3), the organic acid is uniformly mixed with part of water before being added, and then the mixture is added; the organic acid is one or more of formic acid, glacial acetic acid and citric acid.
CN202111318498.2A 2021-11-09 2021-11-09 Hydrophilic elastic silicone oil finishing agent for pure cotton fabric and preparation method thereof Pending CN114000355A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115850711A (en) * 2022-12-23 2023-03-28 广东宏昊化工有限公司 Washable hydrophilic darkening silicone oil and preparation method and finishing agent thereof

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CN110409188A (en) * 2019-08-06 2019-11-05 广东科峰新材料科技有限公司 A kind of hydrophilic soft finishing agent of cotton fabric and preparation method thereof
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CN107814941A (en) * 2017-11-13 2018-03-20 清远市宏图助剂有限公司 A kind of microwave preparation of the quaternized block organosilicon polymer of smooth type
CN110409188A (en) * 2019-08-06 2019-11-05 广东科峰新材料科技有限公司 A kind of hydrophilic soft finishing agent of cotton fabric and preparation method thereof
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