CN110820337A - Ecological fluorine-free waterproof agent and preparation method thereof - Google Patents
Ecological fluorine-free waterproof agent and preparation method thereof Download PDFInfo
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- CN110820337A CN110820337A CN201810920541.4A CN201810920541A CN110820337A CN 110820337 A CN110820337 A CN 110820337A CN 201810920541 A CN201810920541 A CN 201810920541A CN 110820337 A CN110820337 A CN 110820337A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
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Abstract
The invention discloses an ecological fluoride-free waterproofing agent and a preparation method thereof, and the formula comprises: the emulsion comprises octadecyl acrylate, an emulsifier, an initiator and deionized water, wherein the mass percentage of each component is as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water; the preparation method comprises the following steps of firstly, selecting materials; step two, diluting an emulsifier; step three, adding octadecyl acrylate; step four, homogenizing under high pressure; step five, heating and stirring; step six, adding an initiator; step seven, cooling and discharging; the grain size of the waterproof agent is less than 100 microns, the waterproof agent has excellent performance on nylon fabric and good processing stability, can be used as a synergist of a fluorine waterproof agent, has low sensitivity to residual impurities on fabric, is not yellowed when being shaped at the high temperature of 220 ℃ of white yarn dyed fabric, has good durability, does not contain organic halide, fluorocarbon, PFOA, PFOS, APEO and formaldehyde, and is ecological and environment-friendly in preparation method and free of pollution to the environment.
Description
Technical Field
The invention relates to the technical field of textile fabrics, in particular to an ecological fluorine-free waterproof agent and a preparation method thereof.
Background
The history of waterproof finishing of fabrics is long, and China has had waterproof finishing products in the stages of Wei, jin and six dynasties, while the practicability of fluorine-containing alkyl compounds as waterproof and oilproof finishing agents of fabrics is in the 50 th century of 20 th century. In 1950, DuPont (DuPont) in the United states led to Polytetrafluoroethylene (PTFE) emulsions as textile finishes and patented. Subsequently, U.S. 3M company successfully synthesized fluoroalkyl acrylate-containing copolymers for water and oil repellent finishing of fabrics. Since then, more and more water-repellent finishing agents are available and market competition is becoming more and more intense.
The fabric waterproof agent in the current market generally takes fluorine-containing compounds as main materials, but the production and use processes of the fabric waterproof agent have harmful effects on human bodies and the environment, so more and more people put efforts into the research field of fluorine-free fabric waterproof agents; and the export products such as textile fabrics, industrial fabrics and the like have extremely high environmental protection requirements, the products of foreign companies have many problems in the processing process, and the durability and the fabrics can not meet the requirements, so the design of the ecological fluorine-free waterproof agent and the preparation method thereof are necessary.
Disclosure of Invention
The invention aims to provide an ecological fluorine-free waterproof agent and a preparation method thereof, which aim to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: an ecological fluorine-free waterproof agent comprises the following components in percentage by weight: the emulsion comprises octadecyl acrylate, an emulsifier, an initiator and deionized water, wherein the mass percentage of each component is as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water.
A preparation method of an ecological fluorine-free waterproof agent comprises the following steps of selecting materials; step two, diluting an emulsifier; step three, adding octadecyl acrylate; step four, homogenizing under high pressure; step five, heating and stirring; step six, adding an initiator; step seven, cooling and discharging;
in the first step, the components in percentage by mass are as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water, and the octadecyl acrylate, the emulsifier, the initiator and the deionized water are weighed according to the weight percentage sum of 1;
in the second step, the emulsifier and the deionized water are sequentially put into a stirrer and are stirred and diluted uniformly;
in the third step, prepared octadecyl acrylate is put into a reaction vessel and is stirred uniformly;
in the fourth step, the mixture is added into a high-pressure homogenizer for homogenization once, so that the mixture is fully emulsified;
cleaning the reaction kettle with a neutral detergent, drying with hot air until no water stain exists on the inner wall surface of the reaction kettle, adding the homogenized emulsion into the reaction kettle, heating, and stirring;
and in the sixth step, when the temperature reaches 80 ℃, dropwise adding an initiator, continuously stirring for reacting for 8 hours, and then cooling and discharging.
According to the technical scheme, the emulsifier is one or a combination of more of fatty alcohol-polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride.
According to the technical scheme, the initiator is one or a combination of more of azodiisopropyl imidazoline hydrochloride, azodiisobutyronitrile initiator and azodiisoheptanenitrile initiator.
According to the technical scheme, the stirring speed of the stirrer in the second step is 500-650rpm, the stirring time is 8-12min, and the temperature is 45-65 ℃.
According to the technical scheme, the stirring speed of the stirrer in the third step is 300-400rpm, the stirring time is 3-7min, and the temperature is 45-65 ℃.
According to the technical scheme, the speed of the high-pressure homogenizer in the fourth step is 2000-2500rpm, the pressure is 0.5mPa, and the temperature is ambient temperature.
According to the technical scheme, in the fifth step, the drying temperature is not more than 70 ℃, and the drying time is 5-10 min.
According to the technical scheme, after the reaction in the sixth step is finished, the temperature is reduced to the ambient temperature, and then the material is discharged.
Compared with the prior art, the invention has the following beneficial effects: the nylon fabric has the advantages of particle size of less than 100 microns, excellent performance on nylon fabrics, good processing stability, low sensitivity to residual impurities on fabrics, no yellowing during shaping white fabrics at high temperature of 220 ℃, good durability, no organic halide, no fluorocarbon, PFOA, PFOS, APEO and formaldehyde, ecological environmental protection and no pollution to the environment.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution: an ecological fluoride-free waterproof agent and a preparation method thereof:
example 1:
an ecological fluorine-free waterproof agent comprises the following components in percentage by weight: the emulsion comprises octadecyl acrylate, an emulsifier, an initiator and deionized water, wherein the mass percentage of each component is as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water.
A preparation method of an ecological fluorine-free waterproof agent comprises the following steps of selecting materials; step two, diluting an emulsifier; step three, adding octadecyl acrylate; step four, homogenizing under high pressure; step five, heating and stirring; step six, adding an initiator; step seven, cooling and discharging;
in the first step, the components in percentage by mass are as follows: 30% of octadecyl acrylate, 5% of emulsifier, 5% of initiator and 60% of deionized water, and weighing according to the weight percentage sum of 1;
in the second step, the emulsifier and the deionized water are sequentially put into a stirrer, stirred and diluted uniformly, the stirring speed is 650rpm, the stirring time is 8-12min, the temperature is 45-65 ℃, and the emulsifier is one or a combination of more of fatty alcohol-polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride;
in the third step, the prepared octadecyl acrylate is put into a reaction vessel and stirred uniformly, the stirring speed is 300-400rpm, the stirring time is 3-7min, and the temperature is 45-65 ℃;
in the fourth step, the mixture is added into a high-pressure homogenizer for homogenization once, so that the mixture is fully emulsified, the speed is 2000-2500rpm, the pressure is 0.5mPa, and the temperature is ambient temperature;
cleaning the reaction kettle with a neutral detergent, drying with hot air at a drying temperature of no more than 70 ℃ for 5-10min until no water stain exists on the inner wall surface of the reaction kettle, adding the homogenized emulsion into the reaction kettle, heating, and stirring;
and in the sixth step, when the temperature reaches 80 ℃, dropwise adding an initiator, wherein the initiator is one or a combination of more of azodiisopropyl imidazoline hydrochloride, azodiisobutyronitrile initiator and azodiisoheptanenitrile initiator, continuously stirring for reacting for 8 hours, cooling to the ambient temperature, and discharging.
Example 2:
an ecological fluorine-free waterproof agent comprises the following components in percentage by weight: the emulsion comprises octadecyl acrylate, an emulsifier, an initiator and deionized water, wherein the mass percentage of each component is as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water.
A preparation method of an ecological fluorine-free waterproof agent comprises the following steps of selecting materials; step two, diluting an emulsifier; step three, adding octadecyl acrylate; step four, homogenizing under high pressure; step five, heating and stirring; step six, adding an initiator; step seven, cooling and discharging;
in the first step, the components in percentage by mass are as follows: selecting 35% of octadecyl acrylate, 5% of emulsifier, 5% of initiator and 55% of deionized water, and weighing according to the sum of the weight percentages of 1;
in the second step, the emulsifier and the deionized water are sequentially put into a stirrer, stirred and diluted uniformly, the stirring speed is 650rpm, the stirring time is 8-12min, the temperature is 45-65 ℃, and the emulsifier is one or a combination of more of fatty alcohol-polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride;
in the third step, the prepared octadecyl acrylate is put into a reaction vessel and stirred uniformly, the stirring speed is 300-400rpm, the stirring time is 3-7min, and the temperature is 45-65 ℃;
in the fourth step, the mixture is added into a high-pressure homogenizer for homogenization once, so that the mixture is fully emulsified, the speed is 2000-2500rpm, the pressure is 0.5mPa, and the temperature is ambient temperature;
cleaning the reaction kettle with a neutral detergent, drying with hot air at a drying temperature of no more than 70 ℃ for 5-10min until no water stain exists on the inner wall surface of the reaction kettle, adding the homogenized emulsion into the reaction kettle, heating, and stirring;
and in the sixth step, when the temperature reaches 80 ℃, dropwise adding an initiator, wherein the initiator is one or a combination of more of azodiisopropyl imidazoline hydrochloride, azodiisobutyronitrile initiator and azodiisoheptanenitrile initiator, continuously stirring for reacting for 8 hours, cooling to the ambient temperature, and discharging.
Example 3:
an ecological fluorine-free waterproof agent comprises the following components in percentage by weight: the emulsion comprises octadecyl acrylate, an emulsifier, an initiator and deionized water, wherein the mass percentage of each component is as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water.
A preparation method of an ecological fluorine-free waterproof agent comprises the following steps of selecting materials; step two, diluting an emulsifier; step three, adding octadecyl acrylate; step four, homogenizing under high pressure; step five, heating and stirring; step six, adding an initiator; step seven, cooling and discharging;
in the first step, the components in percentage by mass are as follows: selecting 40% of octadecyl acrylate, 5% of emulsifier, 5% of initiator and 50% of deionized water, and weighing according to the sum of the weight percentages of 1;
in the second step, the emulsifier and the deionized water are sequentially put into a stirrer, stirred and diluted uniformly, the stirring speed is 650rpm, the stirring time is 8-12min, the temperature is 45-65 ℃, and the emulsifier is one or a combination of more of fatty alcohol-polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride;
in the third step, the prepared octadecyl acrylate is put into a reaction vessel and stirred uniformly, the stirring speed is 300-400rpm, the stirring time is 3-7min, and the temperature is 45-65 ℃;
in the fourth step, the mixture is added into a high-pressure homogenizer for homogenization once, so that the mixture is fully emulsified, the speed is 2000-2500rpm, the pressure is 0.5mPa, and the temperature is ambient temperature;
cleaning the reaction kettle with a neutral detergent, drying with hot air at a drying temperature of no more than 70 ℃ for 5-10min until no water stain exists on the inner wall surface of the reaction kettle, adding the homogenized emulsion into the reaction kettle, heating, and stirring;
and in the sixth step, when the temperature reaches 80 ℃, dropwise adding an initiator, wherein the initiator is one or a combination of more of azodiisopropyl imidazoline hydrochloride, azodiisobutyronitrile initiator and azodiisoheptanenitrile initiator, continuously stirring for reacting for 8 hours, cooling to the ambient temperature, and discharging.
Based on the above, the nylon fabric has the advantages that the nylon fabric has the particle size of less than 100 microns, excellent performance and good processing stability, can be used as a synergist of a fluorine waterproof agent, has low sensitivity to residual impurities on fabrics, is not yellowed when a white yarn fabric is shaped at a high temperature of 220 ℃, has good durability, does not contain organic halide, fluorocarbon, PFOA, PFOS, APEO and formaldehyde, and is ecological and environment-friendly in preparation method and free of pollution to the environment.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: 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 (9)
1. An ecological fluoride-free waterproof agent is characterized in that: the formula comprises the following components: the emulsion comprises octadecyl acrylate, an emulsifier, an initiator and deionized water, wherein the mass percentage of each component is as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water.
2. A preparation method of an ecological fluorine-free waterproof agent comprises the following steps of selecting materials; step two, diluting an emulsifier; step three, adding octadecyl acrylate; step four, homogenizing under high pressure; step five, heating and stirring; step six, adding an initiator; step seven, cooling and discharging; the method is characterized in that:
in the first step, the components in percentage by mass are as follows: 30-40% of octadecyl acrylate, 2-9% of emulsifier, 2-13% of initiator and 40-60% of deionized water, and the octadecyl acrylate, the emulsifier, the initiator and the deionized water are weighed according to the weight percentage sum of 1;
in the second step, the emulsifier and the deionized water are sequentially put into a stirrer and are stirred and diluted uniformly;
in the third step, prepared octadecyl acrylate is put into a reaction vessel and is stirred uniformly;
in the fourth step, the mixture is added into a high-pressure homogenizer for homogenization once, so that the mixture is fully emulsified;
cleaning the reaction kettle with a neutral detergent, drying with hot air until no water stain exists on the inner wall surface of the reaction kettle, adding the homogenized emulsion into the reaction kettle, heating, and stirring;
and in the sixth step, when the temperature reaches 80 ℃, dropwise adding an initiator, continuously stirring for reacting for 8 hours, and then cooling and discharging.
3. An ecological fluorine-free water repellent according to claim 1, wherein: the emulsifier is one or a combination of fatty alcohol polyoxyethylene ether, dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride.
4. An ecological fluorine-free water repellent according to claim 1, wherein: the initiator is one or the combination of more of azodiisopropyl imidazoline hydrochloride, azodiisobutyronitrile initiator and azodiisoheptanenitrile initiator.
5. The method for preparing an ecological fluorine-free waterproofing agent according to claim 2, wherein: the stirring speed of the stirrer in the second step is 500-650rpm, the stirring time is 8-12min, and the temperature is 45-65 ℃.
6. The method for preparing an ecological fluorine-free waterproofing agent according to claim 2, wherein: the stirring speed of the stirrer in the third step is 300-400rpm, the stirring time is 3-7min, and the temperature is 45-65 ℃.
7. The method for preparing an ecological fluorine-free waterproofing agent according to claim 2, wherein: the speed of the high-pressure homogenizer in the fourth step is 2000-2500rpm, the pressure is 0.5mPa, and the temperature is ambient temperature.
8. The method for preparing an ecological fluorine-free waterproofing agent according to claim 2, wherein: and in the fifth step, the drying temperature is not more than 70 ℃, and the drying time is 5-10 min.
9. The method for preparing an ecological fluorine-free waterproofing agent according to claim 2, wherein: and after the reaction in the sixth step is finished, cooling to the ambient temperature and discharging.
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