CN112694575A - Waterproof coating for textile and preparation process thereof - Google Patents

Waterproof coating for textile and preparation process thereof Download PDF

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Publication number
CN112694575A
CN112694575A CN202011546689.XA CN202011546689A CN112694575A CN 112694575 A CN112694575 A CN 112694575A CN 202011546689 A CN202011546689 A CN 202011546689A CN 112694575 A CN112694575 A CN 112694575A
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Prior art keywords
coating
waterproof coating
solution
parts
textiles
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曹如东
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Huaian Knitted Cap Factory Co ltd
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Huaian Knitted Cap Factory Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • 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
    • C08G77/04Polysiloxanes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof

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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)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to the technical field of waterproof coatings, in particular to a waterproof coating for textiles and a preparation process thereof, wherein the preparation of the waterproof coating needs chemical reagents according to parts by weight, and the preparation process comprises the following steps: hexadecyl trimethoxy silane, methyl triethoxy silane, octamethylcyclotetrasiloxane, potassium hydroxide, silane coupling agent, anionic/nonionic surfactant, butyl acrylate, butyl methacrylate, methyl methacrylate, styrene, hydroxypropyl acrylate and ammonium persulfate. In the embodiment, the resins are subjected to a crosslinking reaction under the action of an initiator to form a complex network structure, so that the crosslinking degree is improved, the structure of the coating is finally more compact, and the performances such as hardness, adhesion and the like are optimized; butyl acrylate and butyl methacrylate used in the experiment are soft monomers, so that the flexibility of the coating can be improved, and the phenomenon of cracking of the coating at low temperature is avoided.

Description

Waterproof coating for textile and preparation process thereof
Technical Field
The invention relates to the technical field of waterproof coatings, in particular to a waterproof coating for textiles and a preparation process thereof.
Background
Clothes, shoes, gloves, and the like, which are common daily goods, are mostly made of fabric. Muddy water of automobile flying petals can pollute clothes and shoes which are just washed, and ice water in winter can infiltrate warm gloves. In the face of the above problems, the fabric seems to become impatient. This is because most of fabrics, such as silk products, hemp products, cotton fabrics, etc., have hydrophilic properties due to a large amount of hydrophilic groups on the surface, and it is necessary for skilled persons to develop waterproof coating products in view of the above problems.
Disclosure of Invention
The invention provides a waterproof coating for textiles and a preparation process thereof, aiming at solving the problem that textiles in the prior art are easily wetted by water.
In order to solve the technical problems, the invention adopts the following technical scheme:
a waterproof coating for textiles, which requires chemical reagents in parts by weight for the preparation of the waterproof coating, comprises:
Figure RE-GDA0002960601230000011
Figure RE-GDA0002960601230000021
a preparation process of a waterproof coating for textiles comprises the following steps:
s1, adding an anionic/nonionic surfactant into a three-neck flask, then sequentially adding deionized water and a proper amount of potassium hydroxide solution, and uniformly stirring for 15-20 min at room temperature to uniformly mix;
s2, evaporating and condensing the solution in the step S1, wherein the heating temperature is 65-75 ℃;
s3, dropwise adding a mixed solution of octamethylcyclotetrasiloxane, methyltriethoxysilane and hexadecyl trimethoxy silane into the solution obtained in the step S2 at a constant speed, reacting at a constant temperature for 8-10 h after the dropwise adding is finished, finally adding a silane coupling agent, and reacting at a constant temperature for 1-2 h to obtain an anionic organic silicon emulsion;
s4, adding anionic organic silicon emulsion and deionized water into a four-neck flask, heating and stirring to fully dissolve the anionic organic silicon emulsion in the deionized water;
s5, weighing monomers of butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, and uniformly mixing in a beaker for later use;
s6, raising the temperature of the solution in the four-neck flask to 80-85 ℃, adding the mixed monomer in the step S5, then slowly dropping an aqueous solution of ammonium persulfate, and continuously reacting for 10-15 minutes;
s7, stirring and cooling to 40-50 ℃, and filtering a product by using gauze;
s8, mixing the product obtained in the step S7, a dispersing agent, a defoaming agent and water-based TiO2And adding zirconium balls into the ball milling tank, ball milling to a standard fineness, and filtering to obtain white uniform slurry.
Preferably, the aqueous solution of ammonium persulfate contains ammonium persulfate in an amount of 10 wt%.
Preferably, the pH of the slurry obtained in S8 is controlled to 6.5 to 8.5.
Preferably, 3 to 8 parts by weight of potassium hydroxide solution are added.
The invention adopts the waterproof coating for the textile and the preparation process thereof, and has the following beneficial effects: in the embodiment, the resins are subjected to a crosslinking reaction under the action of an initiator to form a complex network structure, so that the crosslinking degree is improved, the structure of the coating is finally more compact, and the performances such as hardness, adhesion and the like are optimized; butyl acrylate and butyl methacrylate used in the experiment are soft monomers, so that the flexibility of the coating can be improved, and the phenomenon of cracking of the coating at low temperature is avoided.
Detailed Description
Preparation and Performance characterization of the Water repellent coating
In order to avoid the influence of impurities remaining on the surface of the substrate on various performances of the coating, the glass slide is wiped clean by absolute ethyl alcohol, and after the glass slide is dried in the air, the adjusted waterproof coating is uniformly coated on the surface of the glass slide by a wire rod. Airing for a period of time at room temperature, putting the mixture into an oven, baking and curing at a certain temperature, taking out and cooling, and performing performance test for later use.
1. Gloss: measuring the sample plate by using a KGZ-60 type gloss meter;
2. adhesion force: based on GB/T1720-1979, detecting the coating by a circle drawing method, and judging whether the coating is qualified or not according to the detected grade;
3. water resistance: based on GB/T1773-1979, the sample plate is soaked in water, and after the specified number of days, if the surface layer has no phenomena such as extinction, shedding or foaming, the sample plate is qualified;
4. flexibility: testing the flexibility of the waterproof coating based on GB/T1731-1979;
5. hardness: hardness the hardness of the sample waterproof coating was determined based on GB/T6739-2006.
Example 1
Example 1 discloses a waterproof coating for textiles, which requires the following chemical reagents in parts by weight:
Figure RE-GDA0002960601230000041
a preparation process of a waterproof coating for textiles comprises the following steps:
s1, adding 5 parts of anionic/nonionic surfactant into a three-neck flask, then sequentially adding deionized water and 3 parts of a proper amount of potassium hydroxide solution, and uniformly stirring for 15min at room temperature to uniformly mix;
s2, evaporating and condensing the solution in the step S1, wherein the heating temperature is 65 ℃;
s3, dropwise adding a mixed solution of 5 parts of octamethylcyclotetrasiloxane, 12 parts of methyltriethoxysilane and 11 parts of hexadecyl trimethoxy silane into the solution obtained in the step S2 at a constant speed, reacting at a constant temperature for 8 hours after the dropwise adding is finished, finally adding 4 parts of silane coupling agent, and reacting at a constant temperature for 1 hour to obtain an anionic organic silicon emulsion;
s4, adding anionic organic silicon emulsion and deionized water into a four-neck flask, heating and stirring to fully dissolve the anionic organic silicon emulsion in the deionized water;
s5, weighing 16 parts of monomer butyl methacrylate, 23 parts of butyl acrylate, 4 parts of methyl methacrylate, 3 parts of styrene and 6 parts of hydroxypropyl acrylate in a beaker, and uniformly mixing for later use;
s6, raising the temperature of the solution in the four-neck flask to 80 ℃, adding the mixed monomer in the step S5, then slowly dropping 2 parts of aqueous solution of ammonium persulfate, and continuously reacting for 10 min; wherein, the ammonium persulfate accounts for 10 wt% in the aqueous solution of ammonium persulfate;
s7, stirring and cooling to 40 ℃, and filtering a product by using gauze;
s8, mixing the product obtained in the step S7, a dispersing agent, a defoaming agent and water-based TiO2And adding zirconium balls into the ball milling tank, ball milling to a standard fineness, and filtering to obtain uniform slurry, wherein the pH of the obtained slurry is controlled at 6.5.
Example 2
Example 2 discloses a waterproof coating for textiles, which requires the following chemical reagents in parts by weight:
Figure RE-GDA0002960601230000051
Figure RE-GDA0002960601230000061
a preparation process of a waterproof coating for textiles comprises the following steps:
s1, adding an anionic/nonionic surfactant into a three-neck flask, then sequentially adding deionized water and 5 parts of a proper amount of potassium hydroxide solution, and uniformly stirring at room temperature for 18min to uniformly mix;
s2, evaporating and condensing the solution in the step S1, wherein the heating temperature is 70 ℃;
s3, dropwise adding a mixed solution of 7 parts of octamethylcyclotetrasiloxane, 13 parts of methyltriethoxysilane and 15 parts of hexadecyl trimethoxysilane into the solution in the step S2 at a constant speed, reacting at a constant temperature for 9 hours after the dropwise adding is finished, finally adding 4.5 parts of silane coupling agent, and reacting at a constant temperature for 1.5 hours to obtain an anionic organic silicon emulsion;
s4, adding anionic organic silicon emulsion and deionized water into a four-neck flask, heating and stirring to fully dissolve the anionic organic silicon emulsion in the deionized water;
s5, weighing 22 parts of monomer butyl methacrylate, 28 parts of butyl acrylate, 7 parts of methyl methacrylate, 6 parts of styrene and 14 parts of hydroxypropyl acrylate in a beaker, and uniformly mixing for later use;
s6, raising the temperature of the solution in the four-neck flask to 82 ℃, adding the mixed monomer in the step S5, then slowly dropping 3 parts of aqueous solution of ammonium persulfate, and continuously reacting for 13 minutes; wherein, the ammonium persulfate accounts for 10 wt% in the aqueous solution of ammonium persulfate;
s7, stirring and cooling to 45 ℃, and filtering a product by using gauze;
s8, mixing the product obtained in the step S7, a dispersing agent, a defoaming agent and water-based TiO2And adding zirconium balls into a ball milling tank, ball milling to a standard fineness, and filtering to obtain uniform slurry, wherein the pH of the obtained slurry is controlled at 7.
Example 3
Example 3 discloses a waterproof coating for textiles, which requires the following chemical reagents in parts by weight:
Figure RE-GDA0002960601230000071
a preparation process of a waterproof coating for textiles comprises the following steps:
s1, adding 10 parts of anionic/nonionic surfactant into a three-neck flask, then sequentially adding deionized water and 8 parts of a proper amount of potassium hydroxide solution, and uniformly stirring at room temperature for 20min to uniformly mix;
s2, evaporating and condensing the solution in the step S1, wherein the heating temperature is 75 ℃;
s3, dropwise adding a mixed solution of 8 parts of octamethylcyclotetrasiloxane, 15 parts of methyltriethoxysilane and 18 parts of hexadecyl trimethoxy silane into the solution obtained in the step S2 at a constant speed, reacting at a constant temperature for 10 hours after the dropwise adding is finished, finally adding 5 parts of silane coupling agent, and reacting at a constant temperature for 2 hours to obtain an anionic organic silicon emulsion;
s4, adding anionic organic silicon emulsion and deionized water into a four-neck flask, heating and stirring to fully dissolve the anionic organic silicon emulsion in the deionized water;
s5, weighing 24 parts of monomer butyl methacrylate, 30 parts of butyl acrylate, 10 parts of methyl methacrylate, 9 parts of styrene and 16 parts of hydroxypropyl acrylate in a beaker, and uniformly mixing for later use;
s6, raising the temperature of the solution in the four-neck flask to 85 ℃, adding the mixed monomer in the step S5, then slowly dropping 4 parts of aqueous solution of ammonium persulfate, and continuously reacting for 15 minutes; wherein, the ammonium persulfate accounts for 10 wt% in the aqueous solution of ammonium persulfate;
s7, stirring and cooling to 50 ℃, and filtering a product by using gauze;
s8, mixing the product obtained in the step S7, a dispersing agent, a defoaming agent and water-based TiO2And adding zirconium balls into the ball milling tank, ball milling to a standard fineness, and filtering to obtain white uniform slurry. Wherein the pH of the resulting slurry is controlled to 8.
Results of the experiment
Test items Example 1 Example 2 Example 3
Degree of gloss Milky white and blueLight is not obvious Milk white and blue light are obvious Milky white and blue light is not obvious
Hardness of 1H 3H 1H
Adhesion/grade 1 2 1
Water resistance/(7 d) Slight foaming Qualified Slight foaming
Flexibility/mm 1 2 1
Contact Angle/(°) 120 130 118
From the experimental results, it can be seen that example 2 is the optimum formulation in the present invention, and that the gloss, hardness, adhesion, water resistance, flexibility and contact angle in example 2 are the best in 3 examples.
In the embodiment, the resins are subjected to a crosslinking reaction under the action of an initiator to form a complex network structure, so that the crosslinking degree is improved, the structure of the coating is finally more compact, and the performances such as hardness, adhesion and the like of the coating are optimized.
Butyl acrylate and butyl methacrylate used in the experiment are soft monomers, so that the flexibility of the coating can be improved, and the phenomenon of cracking of the coating at low temperature is avoided.
The contact angle, the hardness, the water resistance and the adhesive force of the coating are all improved along with the increase of the curing temperature, when the temperature reaches 82 ℃, all the performances of the coating are optimal, and when the temperature continues to increase, all the performances of the coating are reduced.
When the curing temperature is lower, the crosslinking reaction is insufficient, the comprehensive performance is poorer, the temperature is raised, the crosslinking degree is favorably improved, the hydrophobic group migration surface is favorably improved, the waterproof performance of the coating is further improved, the comprehensive performance is gradually improved, the overhigh temperature can cause the spreading waste of energy, the appearance of the coating is yellowed, and the overall performance is poorer.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A waterproof coating for textiles, characterized in that the preparation of the waterproof coating requires chemical agents in parts by weight, comprising:
Figure FDA0002855873360000011
2. a preparation process of a waterproof coating for textiles is characterized by comprising the following steps:
s1, adding an anionic/nonionic surfactant into a three-neck flask, then sequentially adding deionized water and a proper amount of potassium hydroxide solution, and uniformly stirring for 15-20 min at room temperature to uniformly mix;
s2, evaporating and condensing the solution in the step S1, wherein the heating temperature is 65-75 ℃;
s3, dropwise adding a mixed solution of octamethylcyclotetrasiloxane, methyltriethoxysilane and hexadecyl trimethoxy silane into the solution obtained in the step S2 at a constant speed, reacting at a constant temperature for 8-10 h after the dropwise adding is finished, finally adding a silane coupling agent, and reacting at a constant temperature for 1-2 h to obtain an anionic organic silicon emulsion;
s4, adding anionic organic silicon emulsion and deionized water into a four-neck flask, heating and stirring to fully dissolve the anionic organic silicon emulsion in the deionized water;
s5, weighing monomers of butyl methacrylate, butyl acrylate, methyl methacrylate, styrene and hydroxypropyl acrylate, and uniformly mixing in a beaker for later use;
s6, raising the temperature of the solution in the four-neck flask to 80-85 ℃, adding the mixed monomer in the step S5, then slowly dropping an aqueous solution of ammonium persulfate, and continuously reacting for 10-15 minutes;
s7, stirring and cooling to 40-50 ℃, and filtering a product by using gauze;
s8, mixing the product obtained in the step S7, a dispersing agent, a defoaming agent and water-based TiO2And adding zirconium balls into the ball milling tank, ball milling to a standard fineness, and filtering to obtain white uniform slurry.
3. A process for preparing a water-repellent coating for textiles as claimed in claim 2, characterised in that ammonium persulfate in aqueous solution of ammonium persulfate accounts for more than 10% by weight.
4. The process for preparing a waterproof coating for textiles according to claim 2, wherein the pH of the slurry obtained in S8 is controlled to 6.5 to 8.5.
5. The process for preparing a waterproof coating for textiles according to claim 2, wherein 3 to 8 parts by weight of potassium hydroxide solution is added.
CN202011546689.XA 2020-12-23 2020-12-23 Waterproof coating for textile and preparation process thereof Pending CN112694575A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103819605A (en) * 2014-03-12 2014-05-28 东华大学 Preparation method for waterproof acrylic ester emulsion finishing agent
CN109054570A (en) * 2018-07-18 2018-12-21 陕西科技大学 A kind of environment protection type high-strength elastic coating and preparation method thereof
CN109591406A (en) * 2018-12-27 2019-04-09 浙江东进新材料有限公司 A kind of waterproof moisture-permeable composite fabric
CN109680522A (en) * 2019-01-11 2019-04-26 辽东学院 A kind of research of silicone modified coating printing paste used for textiles and preparation method
CN111285981A (en) * 2020-03-24 2020-06-16 佛山祺祥合成材料有限公司 Organosilicon modified acrylic emulsion and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103819605A (en) * 2014-03-12 2014-05-28 东华大学 Preparation method for waterproof acrylic ester emulsion finishing agent
CN109054570A (en) * 2018-07-18 2018-12-21 陕西科技大学 A kind of environment protection type high-strength elastic coating and preparation method thereof
CN109591406A (en) * 2018-12-27 2019-04-09 浙江东进新材料有限公司 A kind of waterproof moisture-permeable composite fabric
CN109680522A (en) * 2019-01-11 2019-04-26 辽东学院 A kind of research of silicone modified coating printing paste used for textiles and preparation method
CN111285981A (en) * 2020-03-24 2020-06-16 佛山祺祥合成材料有限公司 Organosilicon modified acrylic emulsion and preparation method thereof

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Application publication date: 20210423