Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defect of poor adsorbability of the existing high-adsorption porous retention aid for papermaking to paper pulp fibers, the preparation method of the high-adsorption porous retention aid for papermaking is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a high-adsorption porous retention aid for papermaking is characterized by comprising the following specific preparation steps:
(1) weighing 24-27 g of shaddock peel, putting the shaddock peel into a beaker, washing the shaddock peel with deionized water, putting the washed shaddock peel into a drying oven for drying, taking out the shaddock peel for grinding and crushing to obtain shaddock peel particles, mixing and stirring the shaddock peel particles and a sodium hydroxide solution with the mass fraction of 21%, taking out for suction filtration, removing filtrate to obtain filter residues, and drying to obtain modified shaddock peel particles;
(2) mixing and soaking flax fibers and a sodium hydroxide solution with the mass fraction of 27% to obtain soaked flax fibers, mixing a silane coupling agent KH-570 and sodium bisulfite, placing the mixture into a four-neck flask provided with a stirrer, a thermometer and a condenser tube, stirring, adding the soaked flax fibers into the four-neck flask after stirring, stirring and refluxing to obtain oxidized flax fibers, washing the oxidized flax fibers with deionized water, finally placing the oxidized flax fibers in an oven for drying, cooling and discharging to obtain modified flax fibers;
(3) mixing 15% by mass of sodium silicate solution and 10mol/L hydrochloric acid, placing the mixture in a beaker, stirring and reacting, washing the mixture with deionized water, heating and reacting to obtain self-made silica sol, and mixing and stirring the self-made silica sol and peach gum to obtain modified self-made silica sol;
(4) respectively weighing modified shaddock peel particles, modified flax fibers, modified self-made silica sol, divinylbenzene, glutamine and deionized water according to parts by weight, mixing, performing ultrasonic dispersion, performing spray drying after ultrasonic dispersion, and collecting dried substances to obtain the high-adsorption porous retention aid for papermaking.
The washing frequency of the step (1) is 3-5, the drying temperature is 70-75 ℃, the drying time is 6-8 min, the crushing time is 15-21 min, and the mass ratio of the shaddock peel particles to the sodium hydroxide solution with the mass fraction of 21% is 1: and 4, mixing and stirring for 16-20 min.
The mass ratio of the flax fibers and the sodium hydroxide solution with the mass fraction of 27% in the step (2) is 1: 7, mixing and soaking for 1-3 h, wherein the mass ratio of the silane coupling agent KH-570 to the sodium bisulfite is 3: 1, the reflux temperature is 120-124 ℃, the reflux time is 3-4 h, the washing times are 3-5 times, the drying temperature is 85-90 ℃, and the drying time is 35-45 min.
The volume ratio of the sodium silicate solution with the mass part of 15% to the hydrochloric acid with the concentration of 10mol/L in the step (3) is 5: 1, stirring reaction is carried out for 25-35 ℃, stirring reaction time is 12-16 min, washing times are 4-6 times, heating temperature rise is 70-80 ℃, stirring reaction time is 1-2 h, and the mass ratio of self-made silica sol to peach gum is 3: 1, mixing and stirring time is 12-15 min.
And (4) respectively weighing 60-80 parts of modified shaddock peel particles, 20-30 parts of modified flax fibers, 20-30 parts of modified self-made silica sol, 1-3 parts of divinylbenzene, 3-5 parts of glutamine and 70-90 parts of deionized water according to parts by weight, wherein the dispersion temperature is 55-65 ℃, the dispersion ultrasonic power is 100-200W, and the dispersion time is 35-40 min.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention utilizes alkaline solution to modify the shaddock peel, is beneficial to removing cutin and waxy layer on the cell wall surface of the shaddock peel, reduces the crystallization and polymerization degree of cellulose, destroys a bonding layer, increases effective specific surface area, is beneficial to improving the adsorbability of the shaddock peel, also utilizes the alkaline solution to destroy chemical bonds among the cellulose, leads the cortex structure to become loose and increases the adsorbability, thereby preparing the retention aid for papermaking, improves the adsorbability of the retention aid for papermaking, utilizes alkaline solution and silane coupling agent KH-570 to modify the surface of flax fiber, wherein the main component of the flax fiber is cellulose, utilizes the alkaline solution to modify the surface of the flax fiber to promote the crystallinity of the cellulose to be improved, is beneficial to improving the mechanical property of the flax fiber, and can increase the surface area of the flax fiber, the adhesion area between the system and the surface of the flax fiber is increased, so that the interface strength between the system and the flax fiber is improved, and the flax fiber contains a large amount of polar functional groups and is modified by using a silane coupling agent KH-570, so that the polar groups of the flax fiber are reduced, the compatibility between the flax fiber and a base material is promoted, and the adsorbability of a retention aid for papermaking is facilitated again;
(2) the invention continuously modifies the silica sol by peach gum with viscosity, and utilizes the modified silica sol with high adsorption activity and viscosity to expose a plurality of hydroxyl and amino matrixes after fermentation reaction, the hydroxyl and amino can be fully close to fibers in paper pulp, the modified silica sol has better film forming capability, simultaneously has enough adhesive strength to the fibers, can bridge among the fibers, has a plurality of positive charge centers and hydroxyl on molecular chains, is convenient to form electrostatic bonding and hydrogen bonds with the fibers, can effectively improve the retention rate of fine fibers and fine materials in the paper pulp, reduces the input of paper pulp raw materials, reduces the consumption of the paper pulp, further improves the adsorption of the retention aid for papermaking, and has wide application prospect.
Detailed Description
Weighing 24-27 g of shaddock peel, putting the shaddock peel into a beaker, washing the shaddock peel with deionized water for 3-5 times, putting the washed shaddock peel into an oven, drying for 6-8 min at the temperature of 70-75 ℃, taking out, grinding and crushing for 15-21 min to obtain shaddock peel particles, and mixing the shaddock peel particles according to the mass ratio of 1: 4, mixing and stirring the shaddock peel particles and a sodium hydroxide solution with the mass fraction of 21% for 16-20 min, taking out, carrying out suction filtration, removing filtrate to obtain filter residues, and drying to obtain modified shaddock peel particles; according to the mass ratio of 1: 7, mixing and soaking flax fibers and 27% sodium hydroxide solution for 1-3 hours to obtain soaked flax fibers, and mixing a silane coupling agent KH-570 and sodium bisulfite according to a mass ratio of 3: 1, mixing and placing the mixture in a four-neck flask provided with a stirrer, a thermometer and a condenser, stirring for 5-7 min, adding soaked flax fibers into the four-neck flask after stirring, stirring and refluxing for 3-4 h at the temperature of 120-124 ℃ to obtain oxidized flax fibers, washing the oxidized flax fibers for 3-5 times by using deionized water, finally placing the mixture in an oven, drying for 35-45 min at the temperature of 85-90 ℃, cooling and discharging to obtain modified flax fibers; according to the volume ratio of 5: 1, mixing 15% by mass of sodium silicate solution and 10mol/L hydrochloric acid, placing the mixture in a beaker, stirring and reacting at 25-35 ℃ for 12-16 min, then washing with deionized water for 4-6 times, heating to 70-80 ℃, and stirring and reacting for 1-2 h to obtain self-prepared silica sol, wherein the mass ratio of the sodium silicate solution to the hydrochloric acid is 3: 1, mixing and stirring the self-made silica sol and peach gum for 12-15 min to obtain modified self-made silica sol; respectively weighing 60-80 parts of modified shaddock peel particles, 20-30 parts of modified flax fibers, 20-30 parts of modified self-made silica sol, 1-3 parts of divinylbenzene, 3-5 parts of glutamine and 70-90 parts of deionized water according to parts by weight, mixing, performing ultrasonic dispersion for 35-40 min at the temperature of 55-65 ℃ and the ultrasonic power of 100-200W, performing spray drying after ultrasonic dispersion, and collecting dried substances to obtain the high-adsorption porous retention aid for papermaking.
Example 1
Weighing 24g of shaddock peel, putting the shaddock peel into a beaker, washing the shaddock peel with deionized water for 3 times, putting the washed shaddock peel into an oven, drying for 6min at the temperature of 70 ℃, taking out, grinding and crushing for 15min to obtain shaddock peel particles, and mixing the particles according to the mass ratio of 1: 4, mixing and stirring the shaddock peel particles and a sodium hydroxide solution with the mass fraction of 21% for 16min, taking out, carrying out suction filtration, removing filtrate to obtain filter residue, and drying to obtain modified shaddock peel particles; according to the mass ratio of 1: 7, mixing and soaking flax fibers and 27% sodium hydroxide solution for 1 hour to obtain soaked flax fibers, and mixing a silane coupling agent KH-570 and sodium bisulfite according to the mass ratio of 3: 1, mixing, placing in a four-neck flask provided with a stirrer, a thermometer and a condenser, stirring for 5min, adding soaked flax fibers into the four-neck flask after stirring, stirring and refluxing for 3h at the temperature of 120 ℃ to obtain oxidized flax fibers, washing the oxidized flax fibers for 3 times by using deionized water, finally placing in a drying oven, drying for 35min at the temperature of 85 ℃, cooling and discharging to obtain modified flax fibers; according to the volume ratio of 5: 1, mixing 15% by mass of sodium silicate solution and 10mol/L hydrochloric acid, placing the mixture in a beaker, stirring and reacting at 25 ℃ for 12min, then washing the mixture for 4 times by using deionized water, heating the mixture to 70 ℃, and stirring and reacting for 1h to obtain self-prepared silica sol, wherein the mass ratio of the sodium silicate solution to the hydrochloric acid is 3: 1, mixing and stirring the self-made silica sol and peach gum for 12min to obtain modified self-made silica sol; respectively weighing 60 parts of modified shaddock peel particles, 20 parts of modified flax fibers, 20 parts of modified self-made silica sol, 1 part of divinylbenzene, 3 parts of glutamine and 70 parts of deionized water according to parts by weight, mixing, performing ultrasonic dispersion for 35min at the temperature of 55 ℃ and the ultrasonic power of 100W, performing spray drying after ultrasonic dispersion, and collecting dried substances to obtain the high-adsorption porous retention aid for papermaking.
Example 2
Weighing 26g of shaddock peel, putting the shaddock peel into a beaker, washing the shaddock peel with deionized water for 4 times, putting the washed shaddock peel into an oven, drying for 7min at the temperature of 72 ℃, taking out, grinding and crushing for 18min to obtain shaddock peel particles, and mixing the particles according to the mass ratio of 1: 4, mixing and stirring the shaddock peel particles and a sodium hydroxide solution with the mass fraction of 21% for 18min, taking out, carrying out suction filtration, removing filtrate to obtain filter residue, and drying to obtain modified shaddock peel particles; according to the mass ratio of 1: 7, mixing and soaking flax fibers and 27% sodium hydroxide solution for 2 hours to obtain soaked flax fibers, and mixing a silane coupling agent KH-570 and sodium bisulfite according to a mass ratio of 3: 1, mixing, placing in a four-neck flask provided with a stirrer, a thermometer and a condenser, stirring for 6min, adding soaked flax fibers into the four-neck flask after stirring, stirring and refluxing for 3.5h at the temperature of 122 ℃ to obtain oxidized flax fibers, washing the oxidized flax fibers for 4 times by using deionized water, finally placing in an oven, drying for 40min at the temperature of 88 ℃, cooling and discharging to obtain modified flax fibers; according to the volume ratio of 5: 1, mixing 15% by mass of sodium silicate solution and 10mol/L hydrochloric acid, placing the mixture in a beaker, stirring and reacting for 14min at the temperature of 30 ℃, washing the mixture for 5 times by using deionized water, heating the mixture to the temperature of 75 ℃, and stirring and reacting for 1.5h to obtain self-prepared silica sol, wherein the mass ratio of the sodium silicate solution to the hydrochloric acid is 3: 1, mixing and stirring the self-made silica sol and peach gum for 14min to obtain modified self-made silica sol; respectively weighing 70 parts of modified shaddock peel particles, 25 parts of modified flax fibers, 25 parts of modified self-made silica sol, 2 parts of divinylbenzene, 4 parts of glutamine and 80 parts of deionized water according to parts by weight, mixing, performing ultrasonic dispersion for 36min at the temperature of 60 ℃ and the ultrasonic power of 150W, performing spray drying after ultrasonic dispersion, and collecting dried substances to obtain the high-adsorption porous retention aid for papermaking.
Example 3
Weighing 27g of shaddock peel, putting the shaddock peel into a beaker, washing the shaddock peel with deionized water for 5 times, putting the washed shaddock peel into an oven, drying for 8min at the temperature of 75 ℃, taking out, grinding and crushing for 21min to obtain shaddock peel particles, and mixing the particles according to the mass ratio of 1: 4, mixing and stirring the shaddock peel particles and a sodium hydroxide solution with the mass fraction of 21% for 20min, taking out, carrying out suction filtration, removing filtrate to obtain filter residue, and drying to obtain modified shaddock peel particles; according to the mass ratio of 1: 7, mixing and soaking flax fibers and 27% sodium hydroxide solution for 3 hours to obtain soaked flax fibers, and mixing a silane coupling agent KH-570 and sodium bisulfite according to the mass ratio of 3: 1, mixing, placing in a four-neck flask provided with a stirrer, a thermometer and a condenser, stirring for 7min, adding soaked flax fibers into the four-neck flask after stirring, stirring and refluxing for 4h at the temperature of 124 ℃ to obtain oxidized flax fibers, washing the oxidized flax fibers for 5 times by using deionized water, finally placing in an oven, drying for 45min at the temperature of 90 ℃, cooling and discharging to obtain modified flax fibers; according to the volume ratio of 5: 1, mixing 15% by mass of sodium silicate solution and 10mol/L hydrochloric acid, placing the mixture in a beaker, stirring and reacting for 16min at 35 ℃, washing the mixture for 6 times by using deionized water, heating the mixture to 80 ℃, and stirring and reacting for 2h to obtain self-prepared silica sol, wherein the mass ratio of the sodium silicate solution to the hydrochloric acid is 3: 1, mixing and stirring the self-made silica sol and peach gum for 15min to obtain modified self-made silica sol; respectively weighing 80 parts of modified shaddock peel particles, 30 parts of modified flax fibers, 30 parts of modified self-made silica sol, 3 parts of divinylbenzene, 5 parts of glutamine and 90 parts of deionized water according to parts by weight, mixing, performing ultrasonic dispersion for 40min at the temperature of 65 ℃ and the ultrasonic power of 200W, performing spray drying after ultrasonic dispersion, and collecting dried substances to obtain the high-adsorption porous retention aid for papermaking.
Comparative example
The retention aid for high-adsorption porous paper making produced by a certain company in Huaian city is used as a comparative example
The high-adsorption porous retention aid for papermaking prepared by the invention and the high-adsorption porous retention aid for papermaking in the comparative example are detected, and the detection results are shown in table 1:
according to the mass ratio of 1:200, stirring and mixing a commercially available retention aid for Basv papermaking with water at the rotating speed of 100r/min for 10min to obtain a retention aid, then adding the obtained retention aid into paper pulp, controlling the addition of the retention aid to be 8% of the mass of the paper pulp, and finally utilizing the paper pulp added with the retention aid to prepare finished paper according to the paper basis weight of 70g/m 2.
The performance of the finished paper made of the retention aid for papermaking obtained in examples 1-3 and the finished paper made of the commercial retention aid for Basv papermaking in the comparative example were tested, and the test results were obtained
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Comparative example |
| Adsorption capacity (mg/g) | 0.16 | 0.17 | 0.19 | 0.11 |
| Retention (%) | 86.6 | 86.8 | 87.8 | 76.2 |
| Paper whiteness (%) | 81.2 | 82.6 | 83.1 | 78.6 |
The data in Table 1 show that the retention aid for papermaking has obvious retention effect, the retention rate of fine fibers and fine materials added into paper pulp is high, meanwhile, the retention aid cannot cause the blockage of a water filtering channel in the using process, the retention aid has the effects of improving the fiber structure of the paper pulp and improving the quality of paper, and the prepared paper has whiteness, is porous and strong in adsorbability, and is obviously superior to the comparative product. Therefore, the method has wide application prospect.