CN110777560A - Softening agent special for softening and mildew prevention of paper and preparation method thereof - Google Patents
Softening agent special for softening and mildew prevention of paper and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/35—Polyalkenes, e.g. polystyrene
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/02—Material of vegetable origin
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
- D21H17/24—Polysaccharides
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
- D21H17/24—Polysaccharides
- D21H17/25—Cellulose
- D21H17/26—Ethers thereof
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/57—Polyureas; Polyurethanes
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/59—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/36—Biocidal agents, e.g. fungicidal, bactericidal, insecticidal agents
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Abstract
The invention relates to the technical field of softening agents, in particular to a softening agent special for softening and mildew prevention of paper and a preparation method thereof, wherein the softening agent comprises the following components in parts by weight: 5-10 parts of resin, 3-8 parts of spermaceti siloxane, 2-5 parts of nano zinc oxide, 2-5 parts of chitosan, 2-4 parts of hydroxyethyl cellulose, 3-5 parts of aloe extract, 1-2 parts of solvent, 1-2 parts of pH regulator, 2-3 parts of liquid wax and 5-10 parts of water, and has the advantages of good hand feeling, good waterproof and mildewproof effects, high stability and no influence on the whiteness of paper.
Description
Technical Field
The invention relates to the technical field of softening agents, in particular to a softening agent special for softening and mildew prevention of paper and a preparation method thereof.
Background
Softening agents are compounds whose molecular structure contains a long-chain hydrocarbon group at one end and a polar or reactive group at the other end that can be bonded to the fiber. Molecules of the softening agent can form outward adsorption of hydrophobic groups on the surface of the fiber, so that the dynamic and static friction factors of the fiber substance are reduced, and smooth and soft hand feeling is obtained. The paper with higher requirement on softness is toilet paper, crepe paper, handkerchief paper, napkin paper and the like, and other paper types such as processed paper have higher requirement on softness, so the application of the softener in papermaking is more and more important.
The action of softeners can be roughly divided into two aspects: firstly, the slippage and the smoothness among the fibers are improved, and the smooth, moist and greasy handfeel is increased. The second is plasticity as plasticizer, namely, plasticity for fixing paper tissue, improving strength and coating adhesive, filling agent and resin. The former is mainly used as a softener in the textile industry, and various softeners can be used according to the type of fibers, the specification of yarns, the knitting method, the use, the fashion style and the like. The paper industry is also widely using softeners because of the current development of paper processing methods that facilitate the use of softeners for treating paper. The latter is a softener selected mainly based on the processing resin, which not only softens the hand of the paper, but also tends to make the fibers easy to slip, soft and elastic, and to enhance the tear strength.
Most of the softening agents are long-chain alkyl organic compounds with l 2-18 (generally l 6-18) carbon atoms, wherein the surfactant accounts for a large proportion. The softening agent molecules can generate softness mainly from long-chain alkyl groups, and the main function of the soluble groups is to enable the soluble groups to dissolve in an aqueous medium and generate a bonding effect with fibers, so that the alkyl groups can generate an orientation effect on the surfaces of the fibers or the periphery of the fibers.
The consumption of disposable household paper such as paper handkerchiefs, toilet paper, napkins and diapers is increasing, the demand for paper quality is also increasing, especially the higher demand for paper softness is provided, so the paper softener is more and more emphasized, the purpose of using the paper softener is that ① reduces the binding force between fibers, reduces the rigidity of paper, reduces the friction force of paper to skin, ② has the function of wetting fiber, improves the smoothness of fiber, increases the smooth and fine feeling of paper, ③ makes paper have plasticity, in a word, the softener can form reverse adsorption of hydrophobic group outward on the surface of fiber, reduces the dynamic and static friction factors of fiber material, and obtains smooth and soft hand feeling.
In daily life, softening agents are required to have not only softening properties but also properties such as mold resistance, water repellency, oil repellency, antistatic properties, and stain release properties.
Paper and various paper products become moldy and damp causing serious losses to individuals, businesses and countries. The mildew process of paper and its product is the irreversible damage of paper product caused by the decrease of mechanical and physical performance. The mold has an influence on the physical properties of the paper, such as folding endurance and tensile strength.
Chinese patent application CN107780299A discloses a mildew-proof and moisture-proof agent for printing paper and a preparation method thereof, which comprises the following raw materials in parts by weight: 20-40 parts of synthetic resin, 2-8 parts of paraffin, 2-6 parts of chitosan and nano TiO
20.5-1 part of polyethylene wax, 2-8 parts of polyethylene wax, 4-10 parts of rosin resin, 0.5-1 part of ethanol, 30-50 parts of deionized water and 1-2 parts of an auxiliary agent. The preparation method comprises the following steps: (1) adding chitosan into deionized water according to the weight part to prepare a solution with the concentration of 4-6% by mass fraction; (2) uniformly stirring and mixing synthetic resin, paraffin, polyethylene wax, rosin resin, ethanol and an auxiliary agent; (3) sequentially adding acetic acid with the concentration of 10 percent by mass fraction, epichlorohydrin and nano TiO
2And (3) uniformly stirring the mixture obtained in the step (2), and oscillating for 10-20min in an ultrasonic oscillator at a constant temperature of 25-28 ℃ to obtain the product. This patent application combines a chitosan natural antimicrobial with nano-TiO
2It has excellent mildew-proof property, fast drying speed, wear resistance, water resistance and water resistance. However, this moisture-proofing agent is only a moisture-proofing agent, and cannot improve the characteristics of paper such as flexibility and whiteness.
Chinese patent CN103866642A discloses a paper softening agent and a preparation method thereof, belonging to the technical field of papermaking. The paper softener comprises the following components in parts by weight: 30-40 parts of sodium polyacrylate, 20-30 parts of starch, 20-30 parts of sodium alginate, 15-20 parts of diisocyanate, 5-15 parts of hexanediol, 5-10 parts of sodium stearate, 5-8 parts of urea and 3-8 parts of citric acid. The paper softener prepared by the patent can ensure that paper has good flexibility and mechanical strength, has certain humidity and has certain cleaning effect. However, this softener only has an effect of improving the flexibility of paper, and cannot improve the characteristics of paper such as mold resistance and whiteness.
At present, the softener with the performances of smoothness, softness and mildew resistance in the market is less, and part of the paper softener has influence on the performances of whiteness, color and light of paper.
Therefore, it is necessary to develop a softening agent for softening and mildew-proof paper and a method for preparing the same, which can solve the above problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the special softening agent for softening and mildew prevention of paper, which has good hand feeling, good waterproof and mildew prevention effects and high stability and has no influence on the whiteness of the paper, and the preparation method thereof.
The invention is realized by the following technical scheme:
a softening agent special for softening and mildew prevention of paper comprises the following components in parts by weight: 5-10 parts of resin, 3-8 parts of spermaceti siloxane, 2-5 parts of nano zinc oxide, 2-5 parts of chitosan, 2-4 parts of hydroxyethyl cellulose, 3-5 parts of aloe extract, 1-2 parts of solvent, 1-2 parts of pH regulator, 2-3 parts of liquid wax and 5-10 parts of water.
Preferably, the resin includes at least one of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyurethane, and ABS.
More preferably, the resin is a mixture of polyethylene and polyurethane.
More preferably, the mass ratio of the polyethylene to the polyurethane is 1-3: 1.
Preferably, the solvent is at least one of isopropanol, propylene glycol and butanediol.
More preferably, the solvent is a mixed solvent of isopropyl alcohol and butylene glycol.
More preferably, the mass ratio of the isopropyl alcohol to the butanediol is 1: 0.5-2.
Preferably, the pH regulator is at least one of acetic acid-sodium acetate buffer solution, ethanol-ammonium acetate buffer solution, citric acid, sorbic acid and sodium bicarbonate.
Preferably, the preparation method of the aloe extract comprises the following steps: drying Aloe, pulverizing, adding organic solvent, ultrasonic extracting, filtering, sequentially extracting the filtrate with ethyl acetate and petroleum ether, concentrating the petroleum ether extractive solution, and drying.
More preferably, the organic solvent is 75-95% ethanol.
More preferably, the organic solvent is dried and pulverized aloe in an amount of 5-8 times the amount of the organic solvent.
More preferably, the time of the ultrasonic extraction is 1-2h, and the ultrasonic power is 100-.
More preferably, the preparation method of the aloe extract comprises the following steps: drying and crushing aloe, adding 5-8 times of 75-95% ethanol, performing ultrasonic extraction for 1-2h with ultrasonic power of 100-.
The invention also relates to a preparation method of the softening agent, which comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and a pH regulator to obtain a solution 1;
(2) adding resin, spermaceti siloxane and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance.
Preferably, the temperature of the ultrasonic is 40-70 ℃, the power is 200-400w, and the time is 2-3 h.
Preferably, the temperature of the microwave is 20-30 ℃, the power is 100-300w, and the time is 0.5-1 h.
More preferably, the preparation method comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and a pH regulator to obtain a solution 1;
(2) adding resin, spermaceti siloxane and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves at 40-70 ℃ and 400w power for 2-3h to obtain a solution 2;
(3) adding nanometer zinc oxide, aloe extract and solvent into the solution 2, and performing microwave-assisted dissolution at 20-30 deg.C with power of 100-.
Preferably, the softening agent also comprises 1-2 parts of surfactant.
More preferably, the surfactant is one or more of sodium dodecyl benzene sulfonate, sodium hexadecyl sulfonate, polyoxyethylene polyol ether, polyoxyethylene fatty alcohol ether and polyoxyethylene nonyl phenol ether.
The invention also relates to a preparation method of the softening agent, which comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and a pH regulator to obtain a solution 1;
(2) adding resin, spermaceti siloxane, a surfactant and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance.
Preferably, the temperature of the ultrasonic is 40-70 ℃, the power is 200-400w, and the time is 2-3 h.
Preferably, the temperature of the microwave is 20-30 ℃, the power is 100-300w, and the time is 0.5-1 h.
More preferably, the preparation method comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and a pH regulator to obtain a solution 1;
(2) adding resin, spermaceti siloxane, a surfactant and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves at 40-70 ℃ and 400w power for 2-3h to obtain a solution 2;
(3) adding nanometer zinc oxide, aloe extract and solvent into the solution 2, and performing microwave-assisted dissolution at 20-30 deg.C with power of 100-.
The softening agent can be used for office paper, wallpaper and the like.
The invention has the beneficial effects that:
the invention combines the resin and the spermaceti siloxane to play a synergistic effect, reduces the mutual friction force among fibers, and effectively improves the softness and the waterproof performance of paper. The flexibility and water-proof performance of the paper are further improved after the surfactant is added.
According to the invention, nano zinc oxide, chitosan and hydroxyethyl cellulose are used in a combined manner, so that the softness of paper is ensured, the antibacterial effect is better, and the stability of the softener is higher.
According to the invention, the aloe is ultrasonically extracted by adopting ethanol, and then ethyl acetate and petroleum ether are sequentially adopted for extraction, so that the obtained aloe extract is added into the softening agent, and after the softening agent is treated, the paper has remarkable softness, water repellency and antibacterial effect, the whiteness of the paper is not influenced, even the whiteness of the paper is improved, and the paper is prevented from yellowing.
The invention limits the adding sequence of all raw materials in the preparation process, firstly prepares chitosan and hydroxyethyl cellulose into solution, and then adds resin, spermaceti siloxane, surfactant and liquid wax into the solution, so that all components are more easily dispersed in the solution and have higher uniformity, and simultaneously prepares the chitosan, the hydroxyethyl cellulose, the resin and the spermaceti siloxane into the solution, and the interaction of the four components in the solution can better enable all the components to play a role and simultaneously improve the stability of the product. Then adding nano zinc oxide, aloe extract and solvent, uniformly diffusing at low temperature, avoiding the inactivation of effective components in the aloe extract, improving the softness of paper, simultaneously improving the antibacterial effect, preventing the paper from yellowing, and ensuring the whiteness of the paper.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1
A softening agent special for softening and mildew prevention of paper comprises the following components in parts by weight: 5 parts of polyethylene, 8 parts of spermaceti siloxane, 5 parts of nano zinc oxide, 5 parts of chitosan, 4 parts of hydroxyethyl cellulose, 5 parts of aloe extract, 2 parts of isopropanol, 1 part of sorbic acid, 3 parts of liquid wax and 10 parts of water.
The preparation method of the aloe extract comprises the following steps: drying and pulverizing Aloe, adding 5 times of 75% ethanol, ultrasonic extracting for 1 hr with ultrasonic power of 100w, filtering, sequentially extracting the filtrate with ethyl acetate and petroleum ether, concentrating the petroleum ether extractive solution, and drying.
The preparation method of the softening agent comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and sorbic acid to obtain a solution 1;
(2) adding resin, spermaceti siloxane and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves at 40 ℃ and 200w for 2 hours to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance at 20 deg.C and power of 100w for 0.5 hr.
Example 2
A softening agent special for softening and mildew prevention of paper comprises the following components in parts by weight: 10 parts of polyurethane, 3 parts of spermaceti siloxane, 2 parts of nano zinc oxide, 2 parts of chitosan, 2 parts of hydroxyethyl cellulose, 3 parts of aloe extract, 1 part of propylene glycol, 2 parts of citric acid, 2 parts of liquid wax and 5 parts of water.
The preparation method of the aloe extract comprises the following steps: drying and crushing aloe, adding 8 times of 95% ethanol, performing ultrasonic extraction for 2h with ultrasonic power of 300w, filtering, sequentially extracting filtrate with ethyl acetate and petroleum ether, concentrating the petroleum ether extract, and drying to obtain the aloe extract.
The preparation method of the softening agent comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and citric acid to obtain a solution 1;
(2) adding resin, spermaceti siloxane and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves at 70 ℃ and 400w for 3 hours to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance at 30 deg.C and power of 300w for 1 hr.
Example 3
A softening agent special for softening and mildew prevention of paper comprises the following components in parts by weight: 8 parts of resin, 5 parts of spermaceti siloxane, 3 parts of nano zinc oxide, 4 parts of chitosan, 3 parts of hydroxyethyl cellulose, 4 parts of aloe extract, 1.5 parts of surfactant, 1.5 parts of solvent, 1.5 parts of sodium bicarbonate, 2.5 parts of liquid wax and 8 parts of water. The resin is a mixture of polyethylene and polyurethane, and the mass ratio of the polyethylene to the polyurethane is 2: 1; the solvent is a mixed solvent of isopropanol and butanediol, and the mass ratio of the isopropanol to the butanediol is 1: 1.
The preparation method of the aloe extract comprises the following steps: drying and pulverizing Aloe, adding 7 times of 85% ethanol, ultrasonic extracting for 1.5 hr with ultrasonic power of 200w, filtering, sequentially extracting the filtrate with ethyl acetate and petroleum ether, concentrating the petroleum ether extractive solution, and drying.
The preparation method of the softening agent comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and sodium bicarbonate to obtain a solution 1;
(2) adding resin, spermaceti siloxane, a surfactant and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves at 55 ℃, the power of 300w and the time of 2.5h to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance at 25 deg.C and power of 200w for 0.75 hr.
Comparative example 1
The difference from the example 3 is only that the nano zinc oxide is replaced by the nano titanium dioxide, and the rest conditions are the same.
Comparative example 2
The only difference from example 3 is that no hydroxyethylcellulose is added, and the other conditions are the same.
Comparative example 3
The only difference from example 3 is that no cetyl siloxane was added, and the other conditions were the same.
Comparative example 4
The difference from example 3 is only that the total mass of the resin is unchanged, the mass ratio of the polyethylene to the polyurethane is 1:2, and the other conditions are the same.
Comparative example 5
The difference from the example 3 is that the total mass of the solvent is unchanged, the mass ratio of the isopropanol to the butanediol is 1:4, and the rest conditions are the same.
Comparative example 6
The difference from example 3 is only that the solvent used in the extraction process of the aloe extract is different, and the rest conditions are the same, specifically as follows:
the preparation method of the aloe extract comprises the following steps: drying and pulverizing Aloe, adding 7 times of 85% ethanol, ultrasonic extracting for 1.5 hr with ultrasonic power of 200w, filtering, sequentially extracting the filtrate with carbon tetrachloride and petroleum ether, concentrating the petroleum ether extractive solution, and drying.
Comparative example 7
The difference from the example 3 is only that the adding sequence of the raw materials in the preparation process of the softening agent is different, and the rest conditions are the same, and the specific steps are as follows:
the preparation method of the softening agent comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and sodium bicarbonate to obtain a solution 1;
(2) adding nano zinc oxide, aloe extract and solvent into the solution 1, and dissolving with microwave assistance at 25 deg.C and power of 200w for 0.75 hr to obtain solution 2;
(3) adding resin, spermaceti siloxane, surfactant and liquid wax into the solution 2, and dissolving with ultrasonic assistance at 55 deg.C and 300w for 2.5 h.
Test example 1
The wallpaper is treated by the softening agents of the examples 1-3 and the comparative examples 1-7, and the specific process comprises the following steps: preparing a softening agent and water into 5 wt% working solution, soaking the paper in the working solution for 30s, and drying at 105 ℃.
Paper hand test, paper softness, smoothness, resilience and bulk were tested for examples 1-3 and comparative examples 1-7, and a control was made without using a softener.
Flexibility test: lightly gripping the single ply paper to assess the softness of the paper;
and (3) testing the slip property: the smoothness of the paper is evaluated by sensing the sliding condition between the paper and the double-layer paper by slightly pushing the double-layer paper;
and (3) resilience testing: the rebound resilience of the folded paper is evaluated by sensing the recovery condition in the loosening process;
testing the filling power: the folded paper was lightly pinched or gripped and the sheet bulk was evaluated by feeling the thickness of the paper.
The hand feeling score is 1-100, wherein 1 is the worst, and 100 is the best, and the final hand feeling score is checked and confirmed after being scored by 4 professional hand feeling evaluators, and the average value is taken.
The test results are shown in table 1.
TABLE 1 test results for example 1-3 and comparative examples 1-7 in terms of hand feel
Test example 2
Wallpaper was treated with softener in the same manner as in test example 1, and tested for whiteness, mold resistance and water resistance, and paper treated without softener was used as a control.
Whiteness degree test method: testing by using a full-automatic whiteness meter tester WSD-3C, averaging 4 points in the front and the back, and recording whiteness data Wg;
the mildew-proof test method comprises the following steps: according to the evaluation of the textile mildew resistance of GB/T24346-2009, the mildew resistance grade is 0-4, the grade 0 is 'no obvious mildew growth under a magnifier', the grade 1 is 'rare or local growth of mildew, the coverage area on the surface of a sample is less than 10%', the grade 2 is 'the coverage area of the mildew on the surface of the sample is less than 30% (10% -30%)', the grade 3 is 'the coverage area of the mildew on the surface of the sample is less than 60% (30-60%)', and the grade 4 is 'the coverage area of the mildew on the surface of the sample reaches or exceeds 60%';
the waterproof test method comprises the following steps: see textile fabric surface moisture resistance determination wetting test (ISO4920:1981), with a rating on the ISO rating of 5-degree formulation;
the results are shown in Table 2.
Table 2 results of whiteness, mold resistance and water resistance tests of examples 1 to 3 and comparative examples 1 to 7
Test example 3
The softeners of example 3 and comparative examples 1-2 and 7 were subjected to the stability test, and the test results are shown in table 3.
The overall stability includes low, medium and high, wherein:
low is the basic safety judgment standard: adjusting pH to 9, stirring at 50 deg.C and 2000r/min for 10min, standing, and observing for 1-7 days.
Medium safety judgment standard: adjusting pH to 10.5, stirring at 70 deg.C and 2000r/min for 20min, standing, and observing for 1-7 days.
High safety judgment standard: adjusting the pH value to 11, stirring for 30min at a constant speed stirrer at 70 ℃ according to 2000r/min, standing and observing for 1-7 days to be stable.
Table 3 softener stability test for example 3 and comparative examples 1-2, 7
The technical scheme of the invention is not limited to the technical scheme disclosed by the technical means, and also comprises the technical scheme formed by any combination of the technical features. While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes may be made in the embodiments without departing from the principles of the invention, and that such changes and modifications are intended to be included within the scope of the invention.
Claims (10)
1. The special softening agent for softening and mildew prevention of paper is characterized by comprising the following components in parts by weight: 5-10 parts of resin, 3-8 parts of spermaceti siloxane, 2-5 parts of nano zinc oxide, 2-5 parts of chitosan, 2-4 parts of hydroxyethyl cellulose, 3-5 parts of aloe extract, 1-2 parts of solvent, 1-2 parts of pH regulator, 2-3 parts of liquid wax and 5-10 parts of water.
2. The softener of claim 1 wherein said resin comprises at least one of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyurethane and ABS, preferably a mixture of polyethylene and polyurethane; the solvent is at least one of isopropanol, propylene glycol and butanediol; the pH regulator is at least one of acetic acid-sodium acetate buffer solution, ethanol-ammonium acetate buffer solution, citric acid, sorbic acid and sodium bicarbonate.
3. The softener of claim 1 wherein said aloe vera extract is prepared by a process comprising the steps of: drying Aloe, pulverizing, adding organic solvent, ultrasonic extracting, filtering, sequentially extracting the filtrate with ethyl acetate and petroleum ether, concentrating the petroleum ether extractive solution, and drying.
4. The softener of claim 3 wherein said aloe extract is prepared by a process comprising the steps of: drying and crushing aloe, adding 5-8 times of 75-95% ethanol, performing ultrasonic extraction for 1-2h with ultrasonic power of 100-.
5. The softener of claim 1 further comprising 1-2 parts of a surfactant.
6. The softener of claim 5 wherein said surfactant is one or more of sodium dodecylbenzene sulfonate, sodium hexadecyl sulfonate, polyoxyethylene polyol ether, polyoxyethylene fatty alcohol ether, polyoxyethylene nonylphenol ether.
7. A process for the preparation of a softener according to any one of claims 1 to 4 comprising the steps of:
(1) mixing chitosan, hydroxyethyl cellulose, water and a pH regulator to obtain a solution 1;
(2) adding resin, spermaceti siloxane and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance.
8. A process for preparing a softener according to claim 5 or 6, characterized in that it comprises the following steps:
(1) mixing chitosan, hydroxyethyl cellulose, water and a pH regulator to obtain a solution 1;
(2) adding resin, spermaceti siloxane, a surfactant and liquid wax into the solution 1, and dissolving with the aid of ultrasonic waves to obtain a solution 2;
(3) adding nanometer zinc oxide, Aloe extract and solvent into solution 2, and dissolving with microwave assistance.
9. The preparation method according to claim 7 or 8, wherein the temperature of the ultrasound is 40-70 ℃, the power is 200-400w, and the time is 2-3 h.
10. The method as claimed in claim 7 or 8, wherein the microwave is at a temperature of 20-30 ℃, a power of 100-300w, and a time of 0.5-1 h.
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