CN111088716A - Preparation method of fixing agent for enhancing uniformity of paper - Google Patents
Preparation method of fixing agent for enhancing uniformity of paper Download PDFInfo
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- CN111088716A CN111088716A CN201911264396.XA CN201911264396A CN111088716A CN 111088716 A CN111088716 A CN 111088716A CN 201911264396 A CN201911264396 A CN 201911264396A CN 111088716 A CN111088716 A CN 111088716A
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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
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
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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
- D21H17/28—Starch
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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
- D21H17/56—Polyamines; Polyimines; Polyester-imides
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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
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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
- D21H21/18—Reinforcing agents
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Abstract
The invention discloses a preparation method of a fixing agent for enhancing the uniformity of paper, belonging to the technical field of pulping and papermaking. The invention utilizes 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to carry out etherification modification on starch, so that active hydroxyl groups on glucose units in the starch are substituted, cationic groups are generated on the surface of the starch, and epoxy groups are introduced, so that the structural complexity of the starch is increased, the starch is subjected to cationic electrostatic adsorption to increase the bonding degree among molecules in the paper pulp, thereby increasing the structural strength of the paper, the invention makes the reed leaves and the corn straws subject to hydrochloric acid soaking and high-temperature and high-pressure alkali liquor reaction to hydrolyze the plant fibers in the reed leaves and the corn straws, meanwhile, in the high-temperature and high-pressure reaction process, fiber molecules are broken to generate fiber molecules with shorter carbon chain length, carboxyl, hydroxyl and other functional group structures are connected into the fiber molecules, and the fiber molecules are easy to adhere to various molecular components in paper by utilizing the functional groups, so that the strength of the fixing agent for the paper is improved.
Description
Technical Field
The invention discloses a preparation method of a fixing agent for enhancing the uniformity of paper, belonging to the technical field of pulping and papermaking.
Background
The proportion of mechanical pulp, chemimechanical pulp and waste paper pulp in the fiber raw material structure of the papermaking industry is increased year by year, and the utilization rate of fibers is greatly improved. With the improvement of a large amount of waste paper pulp, high-yield pulp and white water closed circulation degree in the modern paper making industry, a large amount of dissolved and colloidal substances are gathered in a paper making system, and the pollutants can seriously affect the operation performance of a paper machine, the physical performance of paper and the use effect of a paper making additive.
The dissolved and colloidal substances in the papermaking system are divided into four types according to the source: lignin derivatives, hemicellulose and extractives from pulp raw materials, sticky substances such as adhesives, latex and polymer resins from regenerated fibers, dyes, carboxymethyl cellulose and starch substances from chemical additives, and metal ions (calcium, magnesium and aluminum) and minerals in engineering water. How to effectively remove DCS is an important link for recycling the white water.
Mechanical pulping, however, produces large amounts of fines, lignin and resin extractives; the chemi-mechanical pulp contains anionic hemicellulose, oxidized lignin, resin acid and fatty acid; the waste paper pulp contains stickies such as ink particles, and the stickies form dissolved and colloidal substances with electronegativity, and the accumulation of the stickies brings great adverse effects on the continuous operation of a paper feeder and the paper quality, and simultaneously reduces the use efficiency of other functional paper-making aids and process paper-making aids. How to control dissolution and colloidal substances is an important direction of current chemical research. At present, chemical methods are generally adopted by factories to control dissolved and colloidal substances. The most widely used chemical method is the sticking agent method, which mainly means that inorganic or organic electrolyte with small molecular weight and high positive charge density is used to stick colloid substance and dissolved with strong anion property to paper fiber, and then the paper is taken out of the papermaking system through wet paper sheet forming to purify the system.
Common fixatives include aluminum sulfate, polyaluminum chloride, polydimethyldiallylammonium chloride, polyethyleneimine, polyvinylamine, and the like, all of which have their own advantages. The traditional fixing agent is easy to form a large amount of self-aggregates with pollutants due to too high charge density and too low molecular weight, and enters the circulating white water or is deposited on a paper machine. Additional difficulties are encountered with conventional fixing agents if the white water contains a significant amount of hydrophobic contaminants. For hydrophobic dissolution and colloidal substances (fatty acids, resin acids, coating latexes, adhesives in regenerated fibers, polymer resins, and the like) in the papermaking white water, a fixing agent modified by partial hydrophobization may have a better treatment effect.
However, inorganic aluminum sulfate and polyaluminum chloride are generally not effective as organic polyelectrolytes in medium-alkali papermaking systems; with the increasing exhaustion of petroleum resources, poly dimethyl diallyl ammonium chloride, polyethyleneimine, polyvinylamine and the like based on the petroleum resources inevitably face the problem of being limited by raw materials; and the starch-based fixing agent based on natural polymer modification has relatively convenient and easily obtained raw materials and wide development prospect. And because the starch has unique molecular configuration, the starch-based fixing agent has excellent affinity with carbohydrate dissolving and colloidal substances such as paper pulp fibers, anionic hemicellulose and the like, and can better remove the dissolving and colloidal substances in the pulp. However, the molecular weight of starch is too large, and the high-cationicity starch obtained by direct cationization is easy to cause excessive flocculation of pulp, so that the uniformity and strength of paper are poor.
Therefore, the invention of a fixing agent which does not cause the pulp to be easily flocculated to cause the deterioration of the evenness and strength of the paper is necessary in the technical field of pulping and papermaking.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects that the prior fixing agent causes paper pulp to be easy to flocculate to cause the deterioration of the evenness and the strength of the paper, the preparation method of the fixing agent for enhancing the evenness of the paper is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
the preparation method of the fixing agent for enhancing the evenness of paper comprises the following steps:
adding the modified powdery product, the self-made adhesive, anhydrous methanol and water into a stirrer, stirring at the rotating speed of 1000-1200 r/min for 30-40 min to prepare a pre-prepared solvent, adding polyethyleneimine of which the mass is 10-15% of that of the pre-prepared solvent into the stirrer, and continuously stirring at the rotating speed of 800-1000 r/min for 50-60 min to obtain the fixing agent for enhancing the uniformity of the paper;
the self-made adhesive is prepared by the following specific steps:
(1) putting reed leaves and corn straws into an oven, drying for 12-14 h at the temperature of 60-70 ℃, crushing in a crusher after drying to obtain a mixed product, putting the mixed product and a hydrochloric acid beaker with the mass fraction of 5-9%, putting the beaker into a water bath kettle with the water bath temperature of 10-15 ℃, and standing at constant temperature for 3-4 h to obtain an acidic mixed solution;
(2) adding the acidic mixed solution and 10-15% by mass of sodium hydroxide solution into a reaction kettle, raising the pressure in the reaction kettle to 1.2-1.6 MPa, raising the temperature in the reaction kettle to 180-200 ℃, reacting at constant temperature and constant pressure for 2-3 h to prepare reaction slurry, and dropwise adding 10-20% by mass of sulfuric acid into the reaction kettle to adjust the pH value to 4-5 to prepare a prefabricated reaction solution;
(3) putting the prefabricated reaction liquid and sodium bisulfite into a three-neck flask, placing the three-neck flask into a resistance heating sleeve, installing a condensation reflux pipe into the three-neck flask, raising the temperature in the resistance heating sleeve to 80-100 ℃ for condensation reflux for 2-3 h, dropwise adding 6-10% by mass of sodium hydroxide solution to adjust the pH value to be neutral to prepare an oxidation reaction liquid, putting the oxidation reaction liquid into a rotary evaporator, and concentrating and drying for 2-3 h under the conditions of the rotating speed of 300-360 r/min and the temperature of 50-60 ℃ to prepare a self-made binder;
the specific preparation steps of the modified powdery product are as follows:
(1) putting 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and a sodium hydroxide solution with the mass fraction of 4-6% into a beaker, stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirring device to prepare a reaction solvent, adding starch into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 60-65 ℃, sealing the beaker, and carrying out constant-temperature reaction for 3-4 h to prepare reaction slurry;
(2) putting the reaction slurry and an ethanol solution with the mass fraction of 60-80% into a beaker, stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirrer, pouring into a suction filter for suction filtration to obtain a filter cake, cleaning the filter cake for 3-5 times by using absolute ethanol, putting the filter cake into a vacuum drying oven after cleaning, and drying for 5-7 h under the conditions that the vacuum degree is 100-200 Pa and the temperature is 40-50 ℃ to obtain a modified powdery product.
Preferably, the modified powdery product is 3-5 parts by weight, the self-made adhesive is 2-3 parts by weight, the anhydrous methanol is 5-7 parts by weight, and the water is 6-8 parts by weight.
The mass ratio of the reed leaves to the corn stalks in the specific preparation step (1) of the self-made binder is 1: 10.
The mass ratio of the mixed product in the specific preparation step (1) of the self-made binder to hydrochloric acid with the mass fraction of 5-9% is 1: 10.
the mass ratio of the acidic mixed solution to the sodium hydroxide solution with the mass fraction of 10-15% in the specific preparation step (2) of the self-made binder is 1: 10.
The mass ratio of the prefabricated reaction liquid and the sodium bisulfite in the specific preparation step (3) of the self-made binder is 25: 1.
The mass ratio of the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to the sodium hydroxide solution with the mass fraction of 4-6% in the specific preparation step (1) of the modified powdery product is 1: 20.
the mass of the starch added into the beaker in the specific preparation step (1) of the modified powdery product is 6-10% of the mass of the reaction solvent.
The mass ratio of the reaction slurry to the ethanol solution with the mass fraction of 60-80% in the specific preparation step (2) of the modified powdery product is 1: 5.
The beneficial technical effects of the invention are as follows:
(1) the invention firstly puts 3-chlorine-2-hydroxypropyl trimethyl ammonium chloride into sodium hydroxide solution to be stirred, starch is added into the solution to react at high temperature after stirring to prepare reaction slurry, then the reaction slurry is mixed with ethanol solution to be stirred and reacted, the reaction is carried out, suction filtration, washing and drying are carried out to prepare modified powder product, reed leaves and corn straws are crushed and mixed, the mixture is soaked and mixed with hydrochloric acid, alkali liquor is added into the mixture to carry out high-temperature and high-pressure reaction after the soaking, sulfuric acid is added dropwise into the reaction solution to react, sodium bisulfite is added into the reaction solution to react, self-made binder is prepared after the reaction and concentration, finally the modified powder product, the self-made adhesive, water and other reagents are mixed, polyethyleneimine is added into the mixture to be stirred and discharged to obtain the fixing agent for enhancing the uniformity of paper, active hydroxyl groups on glucose units in the starch are substituted, cationic groups are generated on the surface of the starch, epoxy groups are introduced, so that the structural complexity of the starch is increased, the starch increases the bonding degree among molecules in paper pulp through cationic electrostatic adsorption, so that the structural strength of paper is increased, and meanwhile, the number of functional groups in the starch is increased, so that the intervals among the starches are increased, the fixing agent is difficult to generate flocculation in the paper pulp, and the paper evenness is improved;
(2) according to the invention, reed leaves and corn straws are soaked in hydrochloric acid and react with high-temperature high-pressure alkali liquor, so that plant fibers in the reed leaves and the corn straws are hydrolyzed, meanwhile, fiber molecules are broken to generate fiber molecules with shorter carbon chain length in the high-temperature high-pressure reaction process, carboxyl, hydroxyl and other functional group structures are connected into the fiber molecules, and the fiber molecules are easy to adhere to various molecular components in paper by utilizing the functional groups, so that the strength of the fixing agent for the paper is enhanced, and the application prospect is wide.
Detailed Description
Mixing 3-chloro-2-hydroxypropyl trimethyl ammonium chloride with a sodium hydroxide solution with the mass fraction of 4-6% according to the mass ratio of 1: 20, putting the mixture into a beaker, stirring the mixture for 30 to 40min by using a stirring device at the rotating speed of 500 to 600r/min to prepare a reaction solvent, adding starch accounting for 6 to 10 percent of the mass of the reaction solvent into the beaker, putting the beaker into a water bath kettle with the water bath temperature of 60 to 65 ℃, sealing the beaker, and carrying out constant-temperature reaction for 3 to 4 hours to prepare reaction slurry; putting the reaction slurry and an ethanol solution with the mass fraction of 60-80% into a beaker according to the mass ratio of 1:5, stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirrer, pouring the mixture into a suction filter after stirring for suction filtration to obtain a filter cake, cleaning the filter cake for 3-5 times by using absolute ethanol, putting the cleaned filter cake into a vacuum drying oven, and drying for 5-7 h under the conditions of the vacuum degree of 100-200 Pa and the temperature of 40-50 ℃ to obtain a modified powdery product for later use; putting reed leaves and corn straws into an oven according to a mass ratio of 1:10, drying for 12-14 h at the temperature of 60-70 ℃, putting the dried reed leaves and corn straws into a crusher to be crushed to obtain a mixed product, and mixing the mixed product with 5-9% hydrochloric acid according to a mass ratio of 1:10, putting the beaker into a beaker, putting the beaker into a water bath kettle with the water bath temperature of 10-15 ℃, and standing for 3-4 hours at constant temperature to prepare an acidic mixed solution; adding the acidic mixed solution and a sodium hydroxide solution with the mass fraction of 10-15% into a reaction kettle according to the mass ratio of 1:10, raising the pressure in the reaction kettle to 1.2-1.6 MPa, raising the temperature in the reaction kettle to 180-200 ℃, reacting at constant temperature and constant pressure for 2-3 hours to prepare reaction slurry, and dropwise adding sulfuric acid with the mass fraction of 10-20% into the reaction kettle to adjust the pH value to 4-5 to prepare a prefabricated reaction solution; putting the prefabricated reaction liquid and sodium bisulfite into a three-neck flask according to the mass ratio of 25:1, putting the three-neck flask into a resistance heating sleeve, installing a condensation reflux pipe into the three-neck flask, raising the temperature in the resistance heating sleeve to 80-100 ℃ for condensation reflux for 2-3 h, dropwise adding 6-10% by mass of sodium hydroxide solution to adjust the pH value to be neutral to prepare oxidation reaction liquid, putting the oxidation reaction liquid into a rotary evaporator, and concentrating and drying for 2-3 h under the conditions of the rotating speed of 300-360 r/min and the temperature of 50-60 ℃ to prepare a self-made binder; according to the weight parts, 3-5 parts of a standby modified powdery product, 2-3 parts of the self-made adhesive, 5-7 parts of anhydrous methanol and 6-8 parts of water are put into a stirrer and stirred at the rotating speed of 1000-1200 r/min for 30-40 min to prepare a pre-prepared solvent, polyethyleneimine accounting for 10-15% of the mass of the pre-prepared solvent is added into the stirrer, and stirring is continued at the rotating speed of 800-1000 r/min for 50-60 min to obtain the fixing agent for enhancing the uniformity of paper.
Example 1
Preparation of modified powdered product:
mixing 3-chloro-2-hydroxypropyl trimethyl ammonium chloride with a sodium hydroxide solution with the mass fraction of 4% according to the mass ratio of 1: 20, putting the mixture into a beaker, stirring the mixture for 30min by using a stirring device at the rotating speed of 500r/min to prepare a reaction solvent, adding starch accounting for 6 percent of the mass of the reaction solvent into the beaker, putting the beaker into a water bath kettle with the water bath temperature of 60 ℃, sealing the beaker, and carrying out constant-temperature reaction for 3h to prepare reaction slurry;
putting the reaction slurry and an ethanol solution with the mass fraction of 60% into a beaker according to the mass ratio of 1:5, stirring for 30min at the rotating speed of 500r/min by using a stirrer, pouring the mixture into a suction filter after stirring, carrying out suction filtration to obtain a filter cake, cleaning the filter cake for 3 times by using absolute ethanol, putting the filter cake into a vacuum drying oven after cleaning, and drying for 5 hours under the conditions of the vacuum degree of 100Pa and the temperature of 40 ℃ to obtain a modified powdery product for later use;
preparing a self-made binder:
putting reed leaves and corn straws into an oven according to a mass ratio of 1:10, drying for 12 hours at the temperature of 60 ℃, putting the dried reed leaves and corn straws into a crusher to be crushed to obtain a mixed product, and mixing the mixed product with 5% hydrochloric acid according to a mass ratio of 1:10 putting the beaker into a beaker, putting the beaker into a water bath kettle with the water bath temperature of 10 ℃, and standing for 3 hours at constant temperature to prepare an acidic mixed solution;
adding the acidic mixed solution and a 10% sodium hydroxide solution into a reaction kettle according to the mass ratio of 1:10, raising the pressure in the reaction kettle to 1.2MPa, raising the temperature in the reaction kettle to 180 ℃, reacting for 2 hours at constant temperature and constant pressure to obtain reaction slurry, and dropwise adding 10% sulfuric acid into the reaction kettle to adjust the pH value to 4 to obtain a prefabricated reaction solution;
putting the prefabricated reaction liquid and sodium bisulfite into a three-neck flask according to the mass ratio of 25:1, putting the three-neck flask into a resistance heating sleeve, installing a condensation reflux pipe into the three-neck flask, raising the temperature in the resistance heating sleeve to 80 ℃ for condensation reflux for 2h, dropwise adding 6% by mass of sodium hydroxide solution to adjust the pH value to be neutral to prepare oxidation reaction liquid, putting the oxidation reaction liquid into a rotary evaporator, and concentrating and drying for 2h under the conditions of the rotating speed of 300r/min and the temperature of 50 ℃ to prepare a self-made binder;
preparing a fixing agent for enhancing the evenness of paper:
3 parts of standby modified powdery product, 2 parts of the self-made adhesive, 5 parts of anhydrous methanol and 6 parts of water are put into a stirrer and stirred for 30min at the rotating speed of 1000r/min to prepare a pre-prepared solvent, polyethyleneimine accounting for 10% of the mass of the pre-prepared solvent is added into the stirrer, and stirring is continued at the rotating speed of 800r/min for 50min to obtain the fixing agent for enhancing the uniformity of paper.
Example 2
Preparation of modified powdered product:
mixing 3-chloro-2-hydroxypropyl trimethyl ammonium chloride with a sodium hydroxide solution with the mass fraction of 5% according to the mass ratio of 1: 20, putting the mixture into a beaker, stirring the mixture for 35min by using a stirring device at the rotating speed of 550r/min to prepare a reaction solvent, adding starch accounting for 8 percent of the mass of the reaction solvent into the beaker, putting the beaker into a water bath kettle with the water bath temperature of 62 ℃, sealing the beaker, and carrying out constant-temperature reaction for 3.5h to prepare reaction slurry;
putting the reaction slurry and an ethanol solution with the mass fraction of 70% into a beaker according to the mass ratio of 1:5, stirring for 35min at the rotating speed of 550r/min by using a stirrer, pouring the mixture into a suction filter after stirring, carrying out suction filtration to obtain a filter cake, cleaning the filter cake for 4 times by using absolute ethanol, putting the filter cake into a vacuum drying oven after cleaning, and drying for 6h under the conditions of the vacuum degree of 150Pa and the temperature of 45 ℃ to obtain a modified powdery product for later use;
preparing a self-made binder:
putting reed leaves and corn straws into an oven according to a mass ratio of 1:10, drying for 13h at 65 ℃, putting into a crusher after drying, crushing to obtain a mixed product, and mixing the mixed product with hydrochloric acid with a mass fraction of 7% according to a mass ratio of 1:10 putting the mixture into a beaker, putting the beaker into a water bath kettle with the water bath temperature of 12 ℃, and standing the beaker at constant temperature for 3.5 hours to prepare an acidic mixed solution;
adding the acidic mixed solution and a sodium hydroxide solution with the mass fraction of 12% into a reaction kettle according to the mass ratio of 1:10, raising the pressure in the reaction kettle to 1.4MPa, raising the temperature in the reaction kettle to 190 ℃, reacting for 2.5 hours at constant temperature and constant pressure to obtain reaction slurry, and dropwise adding sulfuric acid with the mass fraction of 15% into the reaction kettle to adjust the pH value to 4 to obtain a prefabricated reaction solution;
putting the prefabricated reaction liquid and sodium bisulfite into a three-neck flask according to the mass ratio of 25:1, putting the three-neck flask into a resistance heating sleeve, installing a condensation reflux pipe into the three-neck flask, raising the temperature in the resistance heating sleeve to 90 ℃ for condensation reflux for 2.5h, dropwise adding a sodium hydroxide solution with the mass fraction of 8% to adjust the pH value to be neutral to prepare an oxidation reaction liquid, putting the oxidation reaction liquid into a rotary evaporator, and concentrating and drying for 2.5h under the conditions of the rotating speed of 330r/min and the temperature of 55 ℃ to prepare a self-made binder;
preparing a fixing agent for enhancing the evenness of paper:
according to the weight portion, 4 portions of the standby modified powdery product, 2 portions of the self-made adhesive, 6 portions of anhydrous methanol and 7 portions of water are put into a stirrer and stirred for 35min at the rotating speed of 1100r/min to prepare the pre-prepared solvent, polyethyleneimine accounting for 12% of the mass of the pre-prepared solvent is added into the stirrer, and the stirring is continued at the rotating speed of 900r/min for 55min to obtain the fixing agent for enhancing the uniformity of paper.
Example 3
Preparation of modified powdered product:
mixing 3-chloro-2-hydroxypropyl trimethyl ammonium chloride with a sodium hydroxide solution with the mass fraction of 6% according to the mass ratio of 1: 20, putting the mixture into a beaker, stirring the mixture for 40min at the rotating speed of 600r/min by using a stirring device to prepare a reaction solvent, adding starch accounting for 10 percent of the mass of the reaction solvent into the beaker, putting the beaker into a water bath kettle with the water bath temperature of 65 ℃, sealing the beaker, and carrying out constant-temperature reaction for 4h to prepare reaction slurry;
putting the reaction slurry and an ethanol solution with the mass fraction of 80% into a beaker according to the mass ratio of 1:5, stirring for 40min at the rotating speed of 600r/min by using a stirrer, pouring the mixture into a suction filter after stirring, carrying out suction filtration to obtain a filter cake, cleaning the filter cake for 5 times by using absolute ethanol, putting the filter cake into a vacuum drying oven after cleaning, and drying for 7h under the conditions of the vacuum degree of 200Pa and the temperature of 50 ℃ to obtain a modified powdery product for later use;
preparing a self-made binder:
putting reed leaves and corn straws into an oven according to a mass ratio of 1:10, drying for 14h at 70 ℃, putting into a crusher after drying, crushing to obtain a mixed product, and mixing the mixed product with 9% hydrochloric acid according to a mass ratio of 1:10 putting the beaker into a beaker, putting the beaker into a water bath kettle with the water bath temperature of 15 ℃, and standing for 4 hours at constant temperature to prepare an acidic mixed solution;
adding the acidic mixed solution and 15% sodium hydroxide solution into a reaction kettle according to the mass ratio of 1:10, raising the pressure in the reaction kettle to 1.6MPa, raising the temperature in the reaction kettle to 200 ℃, reacting for 3 hours at constant temperature and constant pressure to obtain reaction slurry, and dropwise adding 20% sulfuric acid into the reaction kettle to adjust the pH value to 5 to obtain a prefabricated reaction solution;
putting the prefabricated reaction liquid and sodium bisulfite into a three-neck flask according to the mass ratio of 25:1, putting the three-neck flask into a resistance heating sleeve, installing a condensation reflux pipe into the three-neck flask, raising the temperature in the resistance heating sleeve to 100 ℃ for condensation reflux for 3 hours, dropwise adding a sodium hydroxide solution with the mass fraction of 10% to adjust the pH value to be neutral to prepare an oxidation reaction liquid, putting the oxidation reaction liquid into a rotary evaporator, and concentrating and drying for 3 hours under the conditions of the rotating speed of 360r/min and the temperature of 60 ℃ to prepare a self-made binder;
preparing a fixing agent for enhancing the evenness of paper:
according to the weight portion, 5 portions of the standby modified powdery product, 3 portions of the self-made adhesive, 7 portions of anhydrous methanol and 8 portions of water are put into a stirrer and stirred for 40min at the rotating speed of 1200r/min to prepare the pre-prepared solvent, polyethyleneimine with the mass of 15% of the pre-prepared solvent is added into the stirrer, and the stirring is continued at the rotating speed of 1000r/min for 60min to obtain the fixing agent for enhancing the uniformity of paper.
Comparative example 1: essentially the same procedure as in example 2 was followed except that the modified powdered product was absent.
Comparative example 2: essentially the same procedure as in example 2, except that the home-made binder was absent.
Comparative example 3: the fixing agent for enhancing the evenness of paper is produced by Guangzhou company.
And (3) testing the strength of the paper: the fixing agents prepared in the examples and the comparative examples were added to oven dried pulp for papermaking in an amount of 0.4% by mass of the oven dried pulp, and after the addition, the paper was drawn, and then the tensile strength, tear strength, and burst strength were measured.
The tensile strength of the paper was determined according to GB/T453-2002.
The paper tear strength was determined according to GB/T455.1-2002.
The paper burst strength was determined according to GB/T454-2002.
Table 1: results of measuring the Properties of fixing agent
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Tensile Strength (N. m/g) | 30 | 31 | 32 | 19 | 20 | 23 |
| Tear Strength (mN. m)2/g） | 6.2 | 6.3 | 6.5 | 4.0 | 4.2 | 4.5 |
| Burst strength (kPa. m)2/g） | 1.5 | 1.6 | 1.7 | 0.8 | 0.9 | 1.1 |
In summary, it can be seen from table 1 that the fixing agent of the present invention is used in papermaking, and has the advantages of high paper strength, high tensile strength, high tear strength, high bursting strength, good paper uniformity, and wide application prospect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (9)
1. A preparation method of a fixing agent for enhancing the evenness of paper is characterized by comprising the following specific preparation steps:
adding the modified powdery product, the self-made adhesive, anhydrous methanol and water into a stirrer, stirring at the rotating speed of 1000-1200 r/min for 30-40 min to prepare a pre-prepared solvent, adding polyethyleneimine of which the mass is 10-15% of that of the pre-prepared solvent into the stirrer, and continuously stirring at the rotating speed of 800-1000 r/min for 50-60 min to obtain the fixing agent for enhancing the uniformity of the paper;
the self-made adhesive is prepared by the following specific steps:
(1) putting reed leaves and corn straws into an oven, drying for 12-14 h at the temperature of 60-70 ℃, crushing in a crusher after drying to obtain a mixed product, putting the mixed product and a hydrochloric acid beaker with the mass fraction of 5-9%, putting the beaker into a water bath kettle with the water bath temperature of 10-15 ℃, and standing at constant temperature for 3-4 h to obtain an acidic mixed solution;
(2) adding the acidic mixed solution and 10-15% by mass of sodium hydroxide solution into a reaction kettle, raising the pressure in the reaction kettle to 1.2-1.6 MPa, raising the temperature in the reaction kettle to 180-200 ℃, reacting at constant temperature and constant pressure for 2-3 h to prepare reaction slurry, and dropwise adding 10-20% by mass of sulfuric acid into the reaction kettle to adjust the pH value to 4-5 to prepare a prefabricated reaction solution;
(3) putting the prefabricated reaction liquid and sodium bisulfite into a three-neck flask, placing the three-neck flask into a resistance heating sleeve, installing a condensation reflux pipe into the three-neck flask, raising the temperature in the resistance heating sleeve to 80-100 ℃ for condensation reflux for 2-3 h, dropwise adding 6-10% by mass of sodium hydroxide solution to adjust the pH value to be neutral to prepare an oxidation reaction liquid, putting the oxidation reaction liquid into a rotary evaporator, and concentrating and drying for 2-3 h under the conditions of the rotating speed of 300-360 r/min and the temperature of 50-60 ℃ to prepare a self-made binder;
the specific preparation steps of the modified powdery product are as follows:
(1) putting 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and a sodium hydroxide solution with the mass fraction of 4-6% into a beaker, stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirring device to prepare a reaction solvent, adding starch into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 60-65 ℃, sealing the beaker, and carrying out constant-temperature reaction for 3-4 h to prepare reaction slurry;
(2) putting the reaction slurry and an ethanol solution with the mass fraction of 60-80% into a beaker, stirring for 30-40 min at the rotating speed of 500-600 r/min by using a stirrer, pouring into a suction filter for suction filtration to obtain a filter cake, cleaning the filter cake for 3-5 times by using absolute ethanol, putting the filter cake into a vacuum drying oven after cleaning, and drying for 5-7 h under the conditions that the vacuum degree is 100-200 Pa and the temperature is 40-50 ℃ to obtain a modified powdery product.
2. The method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: preferably, the modified powdery product is 3-5 parts by weight, the self-made adhesive is 2-3 parts by weight, the anhydrous methanol is 5-7 parts by weight, and the water is 6-8 parts by weight.
3. The method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the reed leaves to the corn stalks in the specific preparation step (1) of the self-made binder is 1: 10.
4. The method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the mixed product in the specific preparation step (1) of the self-made binder to hydrochloric acid with the mass fraction of 5-9% is 1: 10.
5. the method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the acidic mixed solution to the sodium hydroxide solution with the mass fraction of 10-15% in the specific preparation step (2) of the self-made binder is 1: 10.
6. The method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the prefabricated reaction liquid and the sodium bisulfite in the specific preparation step (3) of the self-made binder is 25: 1.
7. The method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride to the sodium hydroxide solution with the mass fraction of 4-6% in the specific preparation step (1) of the modified powdery product is 1: 20.
8. the method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass of the starch added into the beaker in the specific preparation step (1) of the modified powdery product is 6-10% of the mass of the reaction solvent.
9. The method for preparing the fixing agent for enhancing the formation of paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the reaction slurry to the ethanol solution with the mass fraction of 60-80% in the specific preparation step (2) of the modified powdery product is 1: 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116180327A (en) * | 2023-01-07 | 2023-05-30 | 浙江盛纺纳米材料科技有限公司 | Tensile non-woven fabric and production process thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116180327A (en) * | 2023-01-07 | 2023-05-30 | 浙江盛纺纳米材料科技有限公司 | Tensile non-woven fabric and production process thereof |
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Application publication date: 20200501 |