CN114232381A - Anti-sticking agent for gum dipping process and preparation method thereof - Google Patents
Anti-sticking agent for gum dipping process and preparation method thereof Download PDFInfo
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- CN114232381A CN114232381A CN202111576114.7A CN202111576114A CN114232381A CN 114232381 A CN114232381 A CN 114232381A CN 202111576114 A CN202111576114 A CN 202111576114A CN 114232381 A CN114232381 A CN 114232381A
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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
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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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
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/13—Silicon-containing compounds
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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
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/14—Carboxylic acids; Derivatives 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
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
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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
- D21H17/60—Waxes
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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
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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Abstract
The invention relates to the field of anti-sticking agents, in particular to an anti-sticking agent for a gum dipping process and a preparation method thereof. The invention adopts the organic silicon resin to modify the talcum powder, improves the dispersibility and the hydrophobicity of the talcum powder, forms a protective film through the crosslinking action of the organic silicon resin and has excellent solvent resistance. The invention further mixes the prepared organic silicon resin grafted talcum powder with the cactus ethanol solution, beeswax, emulsifier and pH regulator to prepare the anti-sticking agent for the gum dipping process, and overcomes the defects of low dispersity and easy falling of the talcum powder.
Description
Technical Field
The invention relates to the field of anti-sticking agents, in particular to an anti-sticking agent for a gum dipping process and a preparation method thereof.
Background
With the continuous improvement of the living standard of people, the household paper is one of the most closely consumed goods in the life of people, the production and market demand of the household paper in China is rapidly increased, the quality requirement of people on the household paper is higher and higher, and the development of the paper functionality is followed. In addition to conventional paper such as toilet paper, napkin, book paper, etc., which are required for daily life, paper having more functionalities such as abrasion resistance, high temperature resistance, hydrophobicity, tear resistance, solvent resistance is increasingly in demand and is widely used in various aspects of production and life. The quality of paper directly affects the use condition of consumers, and more enterprises pay attention to the research and development of new products to meet the market demand.
Impregnation is a process for the post-treatment of paper, usually a conventional process for the production of paper with special functionality. The paper is usually dipped into a liquid resin added with some processing aids, and the additives are locked on the surface of the paper by virtue of a cross-linked network formed by the curing of the resin, so that the paper with special functions is obtained. Because of the cohesiveness of the resin, the gummed paper is very easy to adhere to a curing mold, the film forming property of the surface of the paper is affected, and the paper is easy to damage, so that the anti-sticking agent, namely the release agent, is used as a functional substance between the mold and a finished product, plays a role in preventing materials from being stuck to the surface of the mold, and plays a role in the preparation process of the functional paper.
The release agent is a functional processing aid which plays a role in assisting in separation, is arranged between a mold and a formed product and can prevent elastomers such as rubber, resin, plastics and the like and other products made of materials from being stuck on the surface of the mold. In industrial production, in order to weaken adhesion or adsorption between a product and a mold, a release agent is generally coated on the surface of the mold, an interface film layer is formed between the product and a contact surface of the mold, the thickness of the film layer is only in a micron order, the thermal stability is good, a formed effective isolating film can be chemically connected with the surface of the mold, the mold and the product are isolated, and therefore the stripping force is weakened, and a formed part can be rapidly and easily stripped off.
Inorganic release agents have been known for a long time, (e.g. talc powders are used as release agents), the majority of which can be used for production after suitable formulation treatment. However, since the main body of the inorganic release agent is solid, it is relatively difficult and troublesome to use. The inorganic release agent has the advantages of stable chemical performance, basically no reaction with products, low cost, smooth surface of the formed products, less residues and easy painting and finishing. The disadvantages are that the inorganic release agent is difficult to uniformly disperse on the surface of a mould and difficult to coat, and dust particles in the release agent can be scattered in the air when the inorganic release agent is used, so that the inorganic release agent causes harm to human health. The inorganic release agent is less used in the gum dipping process due to the complex operation and the influence of dust dispersion when in use. However, the advantages thereof are apparent, and therefore, development and improvement of an inorganic type release agent are necessary.
CN 107447579A discloses a household paper pulp release agent and a preparation method thereof, wherein the household paper pulp release agent comprises the following components in parts by mass: 40-50 parts of modified vegetable oil, 20-30 parts of beeswax, 10-20 parts of ionic liquid, 10-20 parts of plant ash solution, 5-10 parts of glyceryl stearate, 3-6 parts of polyvinyl alcohol, 2-6 parts of polyethyleneimine, 3-5 parts of bactericide and 5-10 parts of sodium dodecyl sulfate. The vegetable oil is modified, the problems that the vegetable oil has poor oxidation stability and can generate serious oxidation phenomena due to a large amount of carbon-carbon double bonds are solved, and the application range of the vegetable oil is widened.
Disclosure of Invention
Aiming at the defects in the prior art, the invention discloses an anti-sticking agent for a gum dipping process and a preparation method thereof.
An anti-sticking agent for a gum dipping process comprises the following raw materials in parts by mass: 30-40 parts of cactus, 5-15 parts of organic silicon resin grafted talcum powder, 20-30 parts of beeswax, 5-10 parts of emulsifier and 1-2 parts of pH regulator.
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 30-40 parts of cactus are peeled, the meat quality is homogenized for 3-5min at the rotating speed of 8000r/min for 4000-;
(2) heating 20-30 parts of beeswax to 60-80 ℃ according to the mass parts, then adding 5-15 parts of organic silicon resin grafted talcum powder, 30-40 parts of cactus ethanol solution and 5-10 parts of emulsifier, stirring for 5-10min at the rotating speed of 200r/min with the temperature of 70 ℃, finally adding 1-2 parts of pH regulator, continuously stirring for 5-10min at the rotating speed of 200r/min with the temperature of 120-.
The emulsifier is one or a mixture of two or more of glyceryl stearate, tween 80 and polyacrylamide; preferably, the emulsifier is tween 80 and polyacrylamide according to the mass ratio (2-3): (1-2) mixing.
The pH regulator is one of oxalic acid-sodium oxalate buffer solution with pH 6-7 and citric acid-sodium citrate buffer solution with pH 6-7; preferably, the pH adjuster is an oxalic acid-sodium oxalate buffer solution having a pH of 6 to 7.
The preparation method of the organic silicon resin grafted talcum powder comprises the following steps:
s1, adding 5-15 parts of talcum powder and 5-10 parts of vinyltriethoxysilane into 50-80 parts of toluene by mass for ultrasonic treatment for 5-15min, wherein the ultrasonic power is 120-160W and the ultrasonic frequency is 30-60kHz, then placing the mixture at 80-90 ℃ for reaction for 6-8h, centrifuging the mixture for 3-5min at the rotating speed of 8000-12000r/min, and washing and drying the precipitate to obtain the vinyltriethoxysilane grafted talcum powder;
s2, adding 5-15 parts by mass of the vinyltriethoxysilane grafted talcum powder prepared in the step S1 into 30-40 parts by mass of 2 wt% karstedt catalyst solution, stirring for 1-3h at 35-45 ℃, then adding 5-10 parts by mass of triethoxysilane, heating to 90-110 ℃, reacting for 18-24h, centrifuging at the rotation speed of 12000r/min for 3-5min, taking the precipitate, washing and drying to obtain siloxane modified talcum powder;
s3, mixing 4-5 parts of organic silicon and 5-15 parts of siloxane modified talcum powder prepared in the step S2 by mass, uniformly stirring at the rotation speed of 100-200r/min, sequentially adding 10-20 parts of deionized water, 15-30 parts of absolute ethyl alcohol and 0.1-0.5 part of hydrochloric acid, heating to 85 ℃, reacting at the rotation speed of 180r/min for 4-6h, and then decompressing and steaming out low-boiling-point substances at the temperature of 190 ℃ and 15-30kPa to obtain the organic silicon resin grafted talcum powder.
The organic silicon is one or a mixture of 1,1,3, 3-tetramethyl disiloxane and phenyl trimethoxy silane; preferably, the organic silicon is 1,1,3, 3-tetramethyl disiloxane and phenyl trimethoxy silane according to the mass ratio of (1-2): (1-2) mixing.
The invention provides an anti-sticking agent for a gum dipping process, which aims to solve the problems that an inorganic anti-sticking agent is difficult to disperse and easy to fall off and further improve the glossiness and the wear resistance of paper.
Because organic anti-sticking agents are expensive, such as silicone, mineral oil, etc., compared to the low price of paper, organic anti-sticking agents can greatly increase the cost of paper production. The inorganic anti-sticking agent has the problems of difficult dispersion and easy falling, which can cause mechanical loss in production and influence the quality of paper. Therefore, the method for modifying the inorganic anti-sticking agent by using the organic anti-sticking agent combines the advantages of the two anti-sticking agents, makes up for the defects of the inorganic anti-sticking agent, and obtains the novel anti-sticking agent for the gum dipping process with moderate cost.
The invention firstly selects the common antisticking agent talcum powder in industrial production as the base material, the main component of the talcum is talcum hydrous magnesium silicate, and the molecular formula is Mg3[Si4O10](OH)2. The talc powder has excellent physical and chemical properties such as lubricity, fire resistance, acid resistance, insulation, high melting point, chemical inertness, good covering power, softness, good gloss, strong adsorption power and the like, and has a tendency of easily breaking into flakes and special lubricity because the crystal structure of the talc is layered. The method is applied to the papermaking industry, and has the following advantages: 1. the method is beneficial to improving the retention rate of the filler, improving the opacity, smoothness and printability of the paper and endowing the paper with higher ink absorption; 2. the chemical property is stable, and the paper is suitable for papermaking under acidic condition and can also be matched with calcium carbonate for use under neutral condition; 3. it has hydrophobic surfaceThe organic matter is easy to be absorbed on the layered surface, the talcum powder is added, the consumption of dye is reduced, the cost is effectively saved, and in addition, the organic matter can be used as resin, an adhesive inhibitor and a waste paper deinking agent due to lipophilicity; 4. can be well combined with the sizing agent to improve the retention of the sizing agent, reduce the absorptivity of paper sheets and prevent printing ink from penetrating the paper sheets; 5. the talcum powder has a lower friction factor, so that the surface of the coating is smooth and soft, the breakage of the coating can be reduced, the printing pressure is reduced, and the like; 6. as a coating pigment with high aspect ratio, the talcum powder has excellent fiber covering capacity and good printing effect, and can also improve the gravure printing quality; 7. the talcum powder has special lubricating property, and the coated paper made of the talcum powder can obtain high finishing degree on a calender and can reduce the using amount of a lubricant in the coating. However, the resin composition has the same disadvantages as most inorganic release agents, is not highly dispersible, and is easily released.
Therefore, the invention further aims at the existence of the silicon-oxygen bond structure and the surface hydroxyl thereof, and utilizes the principle that the nucleophilicity of the hydroxyl is greater than that of the alkoxy, so that the alkoxy can be replaced, and the silane coupling agent is grafted on the silicon dioxide, and the vinyl triethoxysilane is used for grafting the talcum powder to obtain the talcum powder with the surface containing vinyl bonds; further, by utilizing the principle that a karstedt catalyst catalyzes the addition reaction of vinyl polysiloxane and hydrogen-containing polysiloxane, the triethoxy silane and vinyl on the surface of the talcum powder react to obtain organosilicon capable of participating in organosilicon polymerization reaction; and finally, polymerizing the organosilicon grafted on the surfaces of the 1,1,3, 3-tetramethyldisiloxane, the phenyltrimethoxysilane and the talcum powder by utilizing organosilicon polymerization reaction to obtain the organosilicon resin. Due to the existence of two hydrogen atoms in the 1,1,3, 3-tetramethyl disiloxane, the 1,1,3, 3-tetramethyl disiloxane can easily react with the organic silicon grafted on the surface of the talcum powder and the phenyl trimethoxy silane to form a connecting agent of the 1,1,3, 3-tetramethyl disiloxane and the organic silicon grafted on the surface of the talcum powder; the phenyl group in the phenyl trimethoxy silane can further enhance the hydrophobicity of the prepared organic silicon resin so as to enhance the demolding capacity of the organic silicon resin, and the organic silicon resin is grafted with the talcum powder, so that the talcum powder is not easy to fall off, the polymerization of the talcum powder is reduced, and the dispersibility of the talcum powder is improved.
The cactus extracting solution, namely cactus gel, has been used as a paper making industry for a long time, but the cactus gel is always used as a paper fiber adhesive, and the invention discovers that the cactus gel coated on the surface of paper can play the roles of preventing adhesion and improving the smoothness of the paper, so the invention further adds the cactus extracting solution into the prepared anti-adhesion agent.
The beeswax has the characteristics of anisotropic lubricity, high melting point and chemical resistance, and meanwhile, the beeswax serving as base oil can improve the phase solubility of other components in the release agent. Under proper low concentration, the polyacrylamide solution can be regarded as a net structure, mechanical entanglement and hydrogen bonds among chains form net nodes together, the retention rate of the talcum powder can be improved, and the dispersity of the talcum powder is further improved, and the Tween 80 has good hydrophilic and lipophilic properties and has synergistic effect with polyacrylamide, so that the compatibility of each filler in the prepared anti-sticking agent for the gum dipping process is enhanced, and the dispersing effect of the anti-sticking agent is better.
The invention has the beneficial effects that:
the organic silicon resin grafted talcum powder prepared by the invention can improve the dispersibility and hydrophobicity of the talcum powder, and a protective film is formed by the crosslinking action of the organic silicon resin, so that the organic silicon resin grafted talcum powder has excellent solvent resistance.
The invention further mixes the prepared organic silicon resin grafted talcum powder with the cactus ethanol solution, beeswax, emulsifier and pH regulator to prepare the anti-sticking agent for the gum dipping process, and overcomes the defects of low dispersity and easy falling of the talcum powder.
Detailed Description
Cactus, the variety of which is from Cactus of Mexico in North America, purchased from flower garden of Zhangzhou Longhaibangshan hillside and hillside forests.
Beeswax, cat # stock: 001, cangzhou Jianlin wax industries, Inc.
Polyacrylamide, cat # s: BTJX-003A, Zhejiang Xin environmental protection technology Co.
Talc powder, type: JLD-5050, particle size: 5000 mesh, Jinlingda chemical Co., Ltd, Fushan City.
Vinyltriethoxysilane, cat # s: 8598479, Wuhan Carnoz technologies, Inc.
karstedt catalyst, cat No.: MY 8100, purchased from Anhui Mingyi Si Ltd, prepared as a 2 wt% karstedt catalyst solution using toluene as a solvent.
Triethoxysilane, cat No.: r027300, shanghai yan chemical technology limited.
The concentration of hydrochloric acid used was 36% by weight.
1,1,3, 3-tetramethyldisiloxane, CAS No.: 3277-26-7, cat #: r001012, shanghai yan chemical technology limited; the molecular formula is as follows:
phenyltrimethoxysilane, cat No.: r009881, Shanghai Yi En chemical technology, Inc.
Example 1
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps: heating 25 parts of beeswax to 70 ℃ to melt according to the mass parts, then adding 6 parts of emulsifier to mix, and stirring at the rotating speed of 180r/min for 6min to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
Example 2
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃ to melt according to the mass parts, then adding 35 parts of cactus ethanol solution and 6 parts of emulsifier to mix, and stirring at the rotating speed of 180r/min for 6min to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
Example 3
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃, adding 35 parts of cactus ethanol solution and 6 parts of emulsifier, keeping the temperature at 70 ℃, stirring for 6min at the rotating speed of 180r/min, finally adding 1.4 parts of pH regulator, continuously stirring for 6min at the rotating speed of 180r/min, and cooling to room temperature to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
The pH regulator is oxalic acid-sodium oxalate buffer solution with pH of 6.2.
Example 4
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃, adding 10 parts of organic silicon resin grafted talcum powder, 35 parts of cactus ethanol solution and 6 parts of emulsifier, keeping the temperature at 70 ℃, stirring for 6min at the rotating speed of 180r/min, finally adding 1.4 parts of pH regulator, continuously stirring for 6min at the rotating speed of 180r/min, and cooling to room temperature to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
The pH regulator is oxalic acid-sodium oxalate buffer solution with pH of 6.2.
The preparation method of the organic silicon resin grafted talcum powder comprises the following steps:
s1, adding 10 parts by mass of talcum powder and 8 parts by mass of vinyltriethoxysilane into 60 parts by mass of toluene, carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 150W and the ultrasonic frequency is 40kHz, then placing at 85 ℃ for reaction for 7h, centrifuging at 10000r/min for 4min, washing and drying the precipitate to obtain the vinyltriethoxysilane grafted talcum powder;
s2, adding 10 parts by mass of the vinyl triethoxysilane grafted talcum powder prepared in the step S1 into 35 parts by mass of karstedt catalyst solution with the concentration of 2 wt% and stirring the mixture for 2 hours at 40 ℃, then adding 8 parts by mass of triethoxysilane, heating the mixture to 100 ℃ and reacting the mixture for 20 hours, centrifuging the mixture for 4 minutes at the rotating speed of 10000r/min, taking the precipitate, and washing and drying the precipitate to obtain siloxane modified talcum powder;
s3, mixing 4 parts of organic silicon and 10 parts of siloxane modified talcum powder prepared in the step S2 by mass, uniformly stirring at the rotating speed of 180r/min, sequentially adding 15 parts of deionized water, 20 parts of absolute ethyl alcohol and 0.3 part of hydrochloric acid, heating to 85 ℃, reacting at the rotating speed of 180r/min for 5 hours, and then decompressing and steaming low-boiling-point substances at the temperature of 180 ℃ and under the pressure of 20kPa to obtain the organic silicon resin grafted talcum powder.
The organic silicon is 1,1,3, 3-tetramethyl disiloxane and phenyl trimethoxy silane according to the mass ratio of 1: 1 are mixed.
Example 5
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃, adding 10 parts of organic silicon resin grafted talcum powder, 35 parts of cactus ethanol solution and 6 parts of emulsifier, keeping the temperature at 70 ℃, stirring for 6min at the rotating speed of 180r/min, finally adding 1.4 parts of pH regulator, continuously stirring for 6min at the rotating speed of 180r/min, and cooling to room temperature to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
The pH regulator is oxalic acid-sodium oxalate buffer solution with pH of 6.2.
The preparation method of the organic silicon resin grafted talcum powder comprises the following steps:
s1, adding 10 parts by mass of talcum powder and 8 parts by mass of vinyltriethoxysilane into 60 parts by mass of toluene, carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 150W and the ultrasonic frequency is 40kHz, then placing at 85 ℃ for reaction for 7h, centrifuging at 10000r/min for 4min, washing and drying the precipitate to obtain the vinyltriethoxysilane grafted talcum powder;
s2, adding 10 parts by mass of the vinyl triethoxysilane grafted talcum powder prepared in the step S1 into 35 parts by mass of karstedt catalyst solution with the concentration of 2 wt%, stirring for 2 hours at 40 ℃, then adding 8 parts by mass of triethoxysilane, heating to 100 ℃, reacting for 20 hours, centrifuging at 10000r/min for 4 minutes, taking the precipitate, washing and drying to obtain siloxane modified talcum powder;
s3, mixing 4 parts of organic silicon and 10 parts of siloxane modified talcum powder prepared in the step S2 by mass, uniformly stirring at the rotating speed of 180r/min, sequentially adding 15 parts of deionized water, 20 parts of absolute ethyl alcohol and 0.3 part of hydrochloric acid, heating to 85 ℃, reacting at the rotating speed of 180r/min for 5 hours, and then decompressing and steaming low-boiling-point substances at the temperature of 180 ℃ and under the pressure of 20kPa to obtain the organic silicon resin grafted talcum powder.
The organic silicon is 1,1,3, 3-tetramethyl disiloxane.
Example 6
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃, adding 10 parts of organic silicon resin grafted talcum powder, 35 parts of cactus ethanol solution and 6 parts of emulsifier, keeping the temperature at 70 ℃, stirring for 6min at the rotating speed of 180r/min, finally adding 1.4 parts of pH regulator, continuously stirring for 6min at the rotating speed of 180r/min, and cooling to room temperature to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
The pH regulator is oxalic acid-sodium oxalate buffer solution with pH of 6.2.
The preparation method of the organic silicon resin grafted talcum powder comprises the following steps:
s1, adding 10 parts by mass of talcum powder and 8 parts by mass of vinyltriethoxysilane into 60 parts by mass of toluene, carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 150W and the ultrasonic frequency is 40kHz, then placing at 85 ℃ for reaction for 7h, centrifuging at 10000r/min for 4min, washing and drying the precipitate to obtain the vinyltriethoxysilane grafted talcum powder;
s2 mixing 10 parts by mass of the vinyltriethoxysilane-grafted talc powder prepared in the step S1 and 35 parts by mass of a karstedt catalyst solution having a concentration of 2 wt%, and stirring at 40 ℃ for 2 hours; then, adding 8 parts of triethoxysilane, reacting at 100 ℃ for 20h, centrifuging at 10000r/min for 4min, washing and drying the precipitate to obtain siloxane modified talcum powder;
s3, mixing 4 parts of organic silicon and 10 parts of siloxane modified talcum powder prepared in the step S2 by mass, uniformly stirring at the rotating speed of 180r/min, sequentially adding 15 parts of deionized water, 20 parts of absolute ethyl alcohol and 0.3 part of hydrochloric acid, heating to 85 ℃, reacting at the rotating speed of 180r/min for 5 hours, and then decompressing and steaming low-boiling-point substances at the temperature of 180 ℃ and under the pressure of 20kPa to obtain the organic silicon resin grafted talcum powder.
The organic silicon is phenyl trimethoxy silane.
Comparative example 1
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃, adding 10 parts of talcum powder, 4 parts of organic silicon, 35 parts of cactus ethanol solution and 6 parts of emulsifier, keeping the temperature at 70 ℃, stirring for 6min at the rotating speed of 180r/min, finally adding 1.4 parts of pH regulator, continuously stirring for 6min at the rotating speed of 180r/min, and cooling to room temperature to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
The pH regulator is oxalic acid-sodium oxalate buffer solution with pH of 6.2.
The organic silicon is 1,1,3, 3-tetramethyl disiloxane and phenyl trimethoxy silane according to the mass ratio of 1: 1 are mixed.
Comparative example 2
A preparation method of an anti-sticking agent for a gum dipping process comprises the following steps:
(1) according to the mass parts, 35 parts of cactus are taken to be peeled, the meat quality is homogenized for 4min at the rotating speed of 6000r/min, 55 parts of absolute ethyl alcohol is added, the mixture is stirred for 30min at the rotating speed of 300r/min, and filtering is carried out to obtain the ethanol solution of the cactus;
(2) heating 25 parts of beeswax to 70 ℃, adding 10 parts of siloxane modified talcum powder, 4 parts of organic silicon, 35 parts of cactus ethanol solution and 6 parts of emulsifier, keeping the temperature at 70 ℃, stirring for 6min at the rotating speed of 180r/min, finally adding 1.4 parts of pH regulator, continuously stirring for 6min at the rotating speed of 180r/min, and cooling to room temperature to obtain the anti-sticking agent for the gum dipping process.
The emulsifier is Tween 80 and polyacrylamide according to a mass ratio of 2: 1 are mixed.
The pH regulator is oxalic acid-sodium oxalate buffer solution with pH of 6.2.
The organic silicon is 1,1,3, 3-tetramethyl disiloxane and phenyl trimethoxy silane according to the mass ratio of 1: 1 are mixed.
The preparation method of the siloxane modified talcum powder comprises the following steps:
s1, adding 10 parts by mass of talcum powder and 8 parts by mass of vinyltriethoxysilane into 60 parts by mass of toluene, carrying out ultrasonic treatment for 10min, wherein the ultrasonic power is 150W and the ultrasonic frequency is 40kHz, then placing at 85 ℃ for reaction for 7h, centrifuging at 10000r/min for 4min, washing and drying the precipitate to obtain the vinyltriethoxysilane grafted talcum powder;
s2 mixing 10 parts by mass of the vinyltriethoxysilane-grafted talc powder prepared in the step S1 and 35 parts by mass of a karstedt catalyst solution having a concentration of 2 wt%, and stirring at 40 ℃ for 2 hours; then, 8 parts of triethoxysilane is added into the mixture, the mixture is placed at 100 ℃ for reaction for 20 hours, then the mixture is centrifuged at 10000r/min for 4 minutes, and the precipitate is washed and dried to obtain the siloxane modified talcum powder.
Test example 1
Surface contact angle test:
the anti-sticking agent for the dipping process prepared in each example and comparative example was diluted with water to a concentration of 5 wt%, and then coated on a flat and clean glass slide, and after it was completely cured to form a film at room temperature, the water was dropped on the glass slide, and the contact angle of water on the surface of the mold film was measured by a contact angle measuring instrument. And (3) testing conditions are as follows: three different measurement points are selected for the sample to be measured, the static contact angle of water on the surface of the sample to be measured is measured, and the average value of the three points is adopted. The test results are shown in Table 1.
Table 1: test result of surface contact angle of anti-sticking agent for gum dipping process
| Surface contact Angle/° | |
| Example 1 | 58 |
| Example 2 | 69 |
| Example 3 | 72 |
| Example 4 | 86 |
| Example 5 | 84 |
| Example 6 | 83 |
| Comparative example 1 | 76 |
| Comparative example 2 | 78 |
As can be seen from Table 1, the release agent for the dipping process prepared in example 4 has the largest surface contact angle, which is nearly 90 degrees, which indicates that the release agent has the highest hydrophobicity and also indicates that the release agent has the best anti-blocking effect. Since the release mechanisms of different types of release agents are different, but basically, the release is effectively performed to prevent the product from sticking to the mold, and the quality of the release effect is mainly determined by whether the release agent can form a weak interface layer and the surface tension of the release agent itself. The better the physical properties of the release agent, the better the barrier properties, so the values of the physical properties of the substance whose surface is less wettable can be found from the meaning of the critical surface tension. The more difficult a substance is to wet with other substances, the less critical surface tension it is subjected to. Therefore, the smaller the critical surface tension of the release agent, the better the release performance of the release agent on the mold and the product, and the better the release effect.
Example 1 surface contact angles were less than example 2, indicating that example 2 had a better anti-tack effect due to the effect of the cactus gel to prevent tack and improve paper smoothness. Example 2 the surface contact angle is less than example 3, due to the addition of a pH modifier to example 3, which hydrolyzes a portion of the polysaccharides in the cactus gel, reducing its wettability, and which also enhances the ionic character of the polyacrylamide, enhancing its interaction with the paper fibers. The surface contact angles of the examples 5 and 6 are smaller than that of the example 4, because the existence of two hydrogen atoms in the 1,1,3, 3-tetramethyl disiloxane, the organic silicon grafted on the surface of the talcum powder and the phenyl trimethoxy silane can easily react to form a connecting agent of the two; the phenyl group in the phenyl trimethoxy silane can further enhance the hydrophobicity of the prepared organic silicon resin so as to enhance the demolding capacity of the organic silicon resin, and the organic silicon resin is grafted with the talcum powder, so that the talcum powder is not easy to fall off, the polymerization of the talcum powder is reduced, and the dispersibility of the talcum powder is improved. And 1,1,3, 3-tetramethyl disiloxane or phenyl trimethoxy silane and hydrotalcite surface grafted organosilicon are singly adopted for reaction, 1,1,3, 3-tetramethyl disiloxane is weaker in hydrophobicity, although the reaction is more complete, the hydrophobicity of the final product is not high, and phenyl trimethoxy silane is better in hydrophobicity but is difficult to completely react, so that the hydrophobicity of the obtained product is also poorer. The comparative example 1 can also show that the hydrophobicity is poor due to the fact that the talcum powder is not subjected to surface modification and is poor in dispersibility, and the hydrophobicity is reduced to a certain extent because the organosilicon is not polymerized to form the organosilicon resin.
Test example 2
Solvent resistance test:
sequentially putting the self-made high-temperature-resistant release base paper into Dimethylformamide (DMF) and methyl ethyl ketone solutions for soaking for 10min, then putting the soaked paper sample at room temperature for natural volatilization, observing whether the surface of the paper sample is dissolved or swelled after the solvent in the paper sample is completely volatilized, and if so, indicating that the paper sample is unqualified and otherwise, indicating that the paper sample is qualified.
The gum dipping treatment method comprises the following steps: the anti-sticking agent for the dipping process prepared in each example and comparative example was diluted with water to a concentration of 5 wt%, and then the paper was dipped in a bath ratio of 1 g: and 20mL of the sample paper is immersed into the diluted anti-sticking agent for the gum dipping process, taken out after 5 seconds, placed on a flat plate and dried to obtain the test sample paper.
Table 2: results of paper solvent resistance test
As can be seen from Table 2, examples 4-6 exhibited excellent solvent resistance. This is because the cross-linked network formed by cactus gel, silicone resin grafted talcum powder and polyacrylamide has excellent solvent resistance. The reason why the solvent-resistant effect of the paper treated in example 1 is not satisfactory is that it is difficult to obtain a film capable of completely coating the paper only by using beeswax and an emulsifier, the organic solvent can still permeate the paper until the paper swells, and the beeswax is easily dissolved in dimethylformamide. Polyacrylamide and cactus gels also do not have organic solvent resistance. The invention further aims at the existence of a silicon-oxygen bond structure and hydroxyl on the surface of the silicon-oxygen bond structure, utilizes the principle that the nucleophilicity of the hydroxyl is greater than that of alkoxy to replace alkoxy and graft a silane coupling agent on silicon dioxide, and adopts vinyl triethoxysilane to graft talcum powder to obtain the talcum powder with a vinyl bond on the surface; further, by utilizing the principle that a karstedt catalyst catalyzes the addition reaction of vinyl polysiloxane and hydrogen-containing polysiloxane, the triethoxy silane and vinyl on the surface of the talcum powder react to obtain organosilicon capable of participating in organosilicon polymerization reaction; and finally, polymerizing the organosilicon grafted on the surfaces of the 1,1,3, 3-tetramethyldisiloxane, the phenyltrimethoxysilane and the talcum powder by utilizing organosilicon polymerization reaction to obtain the organosilicon resin. Due to the existence of two hydrogen atoms in the 1,1,3, 3-tetramethyl disiloxane, the 1,1,3, 3-tetramethyl disiloxane can easily react with the organic silicon grafted on the surface of the talcum powder and the phenyl trimethoxy silane to form a connecting agent of the 1,1,3, 3-tetramethyl disiloxane and the organic silicon grafted on the surface of the talcum powder; the phenyl group in the phenyl trimethoxy silane can further enhance the hydrophobicity of the prepared organic silicon resin so as to enhance the demolding capacity of the organic silicon resin, and the organic silicon resin is grafted with the talcum powder, so that the talcum powder is not easy to fall off, the polymerization of the talcum powder is reduced, and the dispersibility of the talcum powder is improved. The organic silicon resin grafted talcum powder prepared by the invention can form a cross-linked network covering the surface of paper due to high dispersibility, the organic silicon resin is connected by a silicon-oxygen bond and has excellent solvent resistance, the talcum powder is used as an inorganic material and is more solvent-resistant, and the cross-linked network formed by the organic silicon resin grafted talcum powder and the talcum powder can greatly protect the paper from being corroded by a solvent. As can be seen from comparative examples 1 and 2, the paper cannot be protected from the organic solvent by directly adding the talcum powder and the organic silicon, because the simple organic silicon does not have solvent resistance, and the talcum powder has poor dispersibility and cannot play a role in protection.
Claims (7)
1. The preparation method of the anti-sticking agent for the gum dipping process is characterized by comprising the following steps:
(1) peeling radix et caulis Opuntiae Dillenii, homogenizing, and extracting with anhydrous ethanol to obtain ethanol solution;
(2) heating and melting beeswax, adding organic silicon resin grafted talcum powder, cactus ethanol solution and emulsifier, mixing, and finally adding a pH regulator to regulate the pH value to obtain the anti-sticking agent for the gum dipping process.
2. The method for preparing the anti-sticking agent for the impregnation process according to claim 1, comprising the steps of:
(1) according to the mass parts, 30-40 parts of cactus are peeled, the meat quality is homogenized for 3-5min at the rotating speed of 8000r/min for 4000-;
(2) heating 20-30 parts of beeswax to 60-80 ℃ according to the mass parts, then adding 5-15 parts of organic silicon resin grafted talcum powder, 30-40 parts of cactus ethanol solution and 5-10 parts of emulsifier, stirring for 5-10min at the rotating speed of 200r/min with the temperature of 70 ℃, finally adding 1-2 parts of pH regulator, continuously stirring for 5-10min at the rotating speed of 200r/min with the temperature of 120-.
3. The method for preparing the anti-sticking agent for the gum dipping process according to claim 2, wherein the emulsifier is one or a mixture of two or more of glyceryl stearate, tween 80 and polyacrylamide.
4. The method of claim 2, wherein the pH adjusting agent is one of oxalic acid-sodium oxalate buffer solution with pH 6-7 and citric acid-sodium citrate buffer solution with pH 6-7.
5. The method for preparing the anti-sticking agent for the gum dipping process according to claim 2, wherein the method for preparing the organic silicon resin grafted talcum powder comprises the following steps:
s1, adding 5-15 parts of talcum powder and 5-10 parts of vinyltriethoxysilane into 50-80 parts of toluene by mass for ultrasonic treatment for 5-15min, wherein the ultrasonic power is 120-160W and the ultrasonic frequency is 30-60kHz, then placing the mixture at 80-90 ℃ for reaction for 6-8h, centrifuging the mixture for 3-5min at the rotating speed of 8000-12000r/min, and washing and drying the precipitate to obtain the vinyltriethoxysilane grafted talcum powder;
s2, adding 5-15 parts by mass of the vinyltriethoxysilane grafted talcum powder prepared in the step S1 into 30-40 parts by mass of 2 wt% karstedt catalyst solution, stirring at 35-45 ℃ for 1-3h, then adding 5-10 parts by mass of triethoxysilane, reacting at 90-110 ℃ for 18-24h, centrifuging at the rotation speed of 12000r/min for 3-5min, taking the precipitate, washing and drying to obtain siloxane modified talcum powder;
s3, mixing 4-5 parts of organic silicon and 5-15 parts of siloxane modified talcum powder prepared in the step S2 by mass, uniformly stirring at the rotation speed of 100-200r/min, sequentially adding 10-20 parts of deionized water, 15-30 parts of absolute ethyl alcohol and 0.1-0.5 part of hydrochloric acid, heating to 85 ℃, reacting at the rotation speed of 180r/min for 4-6h, and then decompressing and steaming out low-boiling-point substances at the temperature of 190 ℃ and 15-30kPa to obtain the organic silicon resin grafted talcum powder.
6. The method for preparing the anti-blocking agent for the dipping process according to claim 5, wherein the organosilicon is one or a mixture of 1,1,3, 3-tetramethyldisiloxane and phenyltrimethoxysilane.
7. An anti-sticking agent for a dipping process, characterized by being prepared by the preparation method of the anti-sticking agent for a dipping process according to any one of claims 1 to 6.
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| CN117327441A (en) * | 2023-09-15 | 2024-01-02 | 苏州佩琦材料科技有限公司 | Electron beam cured high-resistance insulating paint and preparation method thereof |
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