CN115323824A - Process for preparing AKD emulsion based on composite cationic vegetable gum polymer - Google Patents
Process for preparing AKD emulsion based on composite cationic vegetable gum polymer Download PDFInfo
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- CN115323824A CN115323824A CN202210830946.5A CN202210830946A CN115323824A CN 115323824 A CN115323824 A CN 115323824A CN 202210830946 A CN202210830946 A CN 202210830946A CN 115323824 A CN115323824 A CN 115323824A
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- 229920000642 polymer Polymers 0.000 title claims abstract description 47
- 125000002091 cationic group Chemical group 0.000 title claims abstract description 42
- 239000000839 emulsion Substances 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 229920001938 Vegetable gum Polymers 0.000 title claims description 32
- 239000000843 powder Substances 0.000 claims abstract description 70
- 241000196324 Embryophyta Species 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 150000001768 cations Chemical class 0.000 claims abstract description 38
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011347 resin Substances 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 32
- 239000003513 alkali Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 claims abstract description 7
- 108010015133 Galactose oxidase Proteins 0.000 claims abstract description 7
- 229920002907 Guar gum Polymers 0.000 claims abstract description 7
- 239000000665 guar gum Substances 0.000 claims abstract description 7
- 229960002154 guar gum Drugs 0.000 claims abstract description 7
- 235000010417 guar gum Nutrition 0.000 claims abstract description 7
- 244000275012 Sesbania cannabina Species 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000005303 weighing Methods 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 20
- 238000007599 discharging Methods 0.000 claims description 20
- 239000012153 distilled water Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000003995 emulsifying agent Substances 0.000 claims description 17
- -1 polytetrafluoroethylene Polymers 0.000 claims description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 235000013311 vegetables Nutrition 0.000 claims description 15
- 230000001804 emulsifying effect Effects 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 10
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 239000003381 stabilizer Substances 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims description 6
- 229930182490 saponin Natural products 0.000 claims description 6
- 150000007949 saponins Chemical class 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 229920002472 Starch Polymers 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 239000011790 ferrous sulphate Substances 0.000 claims description 5
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229940015043 glyoxal Drugs 0.000 claims description 5
- 125000006038 hexenyl group Chemical group 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 229940037312 stearamide Drugs 0.000 claims description 5
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 5
- CSPHGSFZFWKVDL-UHFFFAOYSA-M (3-chloro-2-hydroxypropyl)-trimethylazanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC(O)CCl CSPHGSFZFWKVDL-UHFFFAOYSA-M 0.000 claims description 3
- 108090000790 Enzymes Proteins 0.000 claims description 2
- 102000004190 Enzymes Human genes 0.000 claims description 2
- 239000007957 coemulsifier Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000004513 sizing Methods 0.000 abstract description 23
- RUUHDEGJEGHQKL-UHFFFAOYSA-M 2-hydroxypropyl(trimethyl)azanium;chloride Chemical compound [Cl-].CC(O)C[N+](C)(C)C RUUHDEGJEGHQKL-UHFFFAOYSA-M 0.000 abstract description 4
- 239000000460 chlorine Substances 0.000 abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 4
- 229920001131 Pulp (paper) Polymers 0.000 abstract description 2
- 238000010559 graft polymerization reaction Methods 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 239000003292 glue Substances 0.000 abstract 3
- 241000931143 Gleditsia sinensis Species 0.000 abstract 1
- 235000013399 edible fruits Nutrition 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 35
- 239000000123 paper Substances 0.000 description 8
- 241000219782 Sesbania Species 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004026 adhesive bonding Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011087 paperboard Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- D21H21/16—Sizing or water-repelling agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/12—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated acetals or ketals
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/20—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to the technical field of AKD emulsion preparation processes, and provides a process for preparing AKD emulsion based on a composite cationic plant gum polymer, wherein plant gum (namely Chinese honeylocust fruit gum powder, sesbania gum powder and guar gum powder) is modified by galactose oxidase and mannose, so that the glue applying lag of AKD can be improved, the glue applying efficiency of the AKD emulsion can be improved, and a large amount of cations can be carried in the plant gum through the reaction with 3-chlorine, 2-hydroxypropyl trimethyl ammonium chloride and alkali liquor, so that the emulsified AKD emulsion has more positive charges, and the positive charges can be mutually attracted with negative charges in paper pulp fibers in the paper making glue applying process, thereby improving the retention rate of AKD on the paper fibers; the polymer emulsified AKD formed by graft polymerization of the acetaldehyde resin and the cation modified plant rubber powder can improve the water resistance of paper after sizing and can quickly achieve quick curing after sizing, so that the sizing stability of the AKD can be improved, and the performance of paper processed and produced after the AKD is sized is enhanced.
Description
Technical Field
The invention relates to the technical field of AKD emulsion preparation processes, and particularly relates to a process for preparing AKD emulsion based on a composite cationic vegetable gum polymer.
Background
The surface sizing agent products applied to the domestic market at present mainly comprise 2 kinds of styrene-acrylic surface sizing agents and AKD reactive surface sizing agents, wherein the styrene-acrylic surface sizing agents are mainly applied to large-scale paperboard production lines and are suitable for large-scale production lines with higher surface smoothness and clean slurry treatment, reaction time is not needed after the products are off-line, and the water-resistant effect is better; the AKD sizing agent is suitable for medium and small production lines with poor surface smoothness of paper sheets, incomplete pulp treatment and poor cleanliness, but needs a certain reaction time after the production line is taken out. The class 2 surface sizing agent has certain limitation in application, and has certain defects in application performance and action effect, and the class 2 sizing agent composite sizing agent is applied to the market, but expected effects (sizing instantaneity and high water resistance) cannot be reflected perfectly in the presence of complex and changeable production environments. Therefore, the development of a surface sizing agent with a brand-new concept is an urgent need in the chemical industry of papermaking, namely the surface sizing agent is required to be wider in application range, so that the surface sizing agent has high water resistance and obvious quick curing effect, and the cost of the surface sizing agent can be lower.
Disclosure of Invention
Solves the technical problem
Aiming at the defects of the prior art, the invention provides a process for preparing AKD emulsion based on a composite cationic vegetable gum polymer, aiming at enabling the prepared AKD emulsion to have high water resistance and quick curing effect.
Technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a process for preparing AKD emulsion based on composite cationic vegetable gum polymer comprises the following preparation steps:
s1, adding alkali liquor into a reaction kettle, then adding 28-30 parts of saponin rubber powder, 25-28 parts of sesbania rubber powder and 35-40 parts of guar gum powder under the stirring condition of 300-400rpm, adding galactose oxidase and mannose enzyme when the stirring speed is increased to 600-800rpm, reacting for 3-4 hours at 120-130 ℃ after uniform dispersion, pouring the obtained product into an ethanol water solution to adjust the pH value to 7, filtering out supernate, washing precipitate by using the ethanol water solution, drying and crushing to obtain modified plant rubber powder;
s2, weighing 100 parts of modified plant gum powder in S1, putting the modified plant gum powder into a clean and dry reaction kettle, spraying alkali liquor into the kettle under the condition of stirring, reacting for 25-30min at 50 ℃, spraying a mixture of an etherifying agent and the alkali liquor, reacting for 3-4h at 65 ℃, discharging, washing and soaking a discharged product for two times by using 60% ethanol, soaking and washing for 30min by using absolute ethanol, and performing suction filtration and drying to obtain the cationic modified plant gum powder;
s3, weighing 30 parts of oxidized cation modified plant rubber powder, slowly adding the oxidized cation modified plant rubber powder into a container filled with 60 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, starting the electric stirrer, adding a self-made acetaldehyde resin solution, heating to 60 ℃, adding 0.3 part of sodium dodecyl sulfate and 1 part of tributyl phosphate, and stirring and emulsifying for 30min;
s4, adding 5-8 parts of ammonium sulfate and 7-8 parts of vinyl acetate into the system in the S3, reacting for 30min, heating to 70 ℃, then dropwise adding 18 parts of vinyl acetate again, after dropwise adding is completed within 3h, heating to 80 ℃, preserving heat for 30min, then adding 0.2 part of sodium thiosulfate, finally heating to 90 ℃, preserving heat for 30min, cooling, discharging, and then using a viscosity stabilizer to adjust viscosity, thus obtaining the cationic modified vegetable gum-acetaldehyde resin polymer;
s5, weighing 200 parts of AKD and 100 parts of deionized water, adding the AKD and the deionized water into a three-neck flask, stirring, heating to completely melt the AKD and the deionized water at 60 ℃, increasing the rotation speed, adding 25-28 parts of the cation modified vegetable gum-acetaldehyde resin polymer in S4 and 10-15 parts of the auxiliary emulsifier, premixing for 5min, and transferring the mixture into a homogenizer;
s6, adding 3-5 parts of dispersing agent into a system in a homogenizer in S5, uniformly mixing, performing high-speed shearing emulsification for 10-20min at a rotating speed of 10000r/min by using a high-shear emulsifying machine, cooling to room temperature, adding 13-15 parts of polyaluminum chloride, and uniformly mixing to obtain the AKD emulsion based on the composite cationic vegetable gum polymer.
Furthermore, the alkali liquor in S1 and S2 is prepared 4% sodium hydroxide solution.
Further, the total mass of the two alkali liquors in the S2 is 30% of the total system mass.
Further, the etherifying agent in the S2 is 3-chloro, 2-hydroxypropyl trimethyl ammonium chloride, and the mass of the etherifying agent is 40% of the total system mass.
Furthermore, the method for modifying the plant rubber powder by oxidizing the cations in the S3 comprises the following steps: weighing 50 parts of cation modified plant rubber powder in S2, slowly adding the cation modified plant rubber powder into a container filled with 100 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant pressure funnel, then adding 0.1 part of ferrous sulfate at 50 ℃, slowly dropwise adding 3 parts of hydrogen peroxide, oxidizing for 15-20min, then adding 0.3 part of sodium thiosulfate, standing for 30min, discharging, performing suction filtration by a sand core funnel, washing and drying to obtain the oxidized cation modified plant rubber powder.
Further, the stirring speed is 400-500r/min, and the dropping speed of dropping hydrogen peroxide is 1-2 drops/s.
Further, the preparation method of the acetaldehyde resin solution in S4 comprises the following steps:
step 1, weighing 20g of polyvinyl alcohol and 150mL of distilled water, adding the polyvinyl alcohol and the distilled water into a three-opening beaker with a spherical condenser tube, a polytetrafluoroethylene electric stirrer and a constant-pressure funnel, standing for 30min, starting the electric stirrer, and preserving heat at 95 ℃ for 30min until the polyvinyl alcohol is completely dissolved;
and 2, cooling the system in the step 1 to 70 ℃, adjusting the pH to 3-4 by using a hydrochloric acid solution, dripping 6mL of glyoxal within 30min, keeping the temperature for 1h after dripping is finished, adjusting the pH to be neutral by using a sodium hydroxide solution, cooling and discharging to obtain the acetaldehyde resin solution.
Further, the mass of the viscosity stabilizer in S4 is 3% of the total system mass, and the viscosity of the cation-modified vegetable gum-acetaldehyde resin polymer in S4 is 2800 to 2900mPa · S.
Further, the coemulsifier in S5 is a starch emulsifier.
Still further, the dispersant in S6 is hexenyl bis stearamide.
Advantageous effects
The invention provides a process for preparing AKD emulsion based on a composite cationic vegetable gum polymer, which has the following beneficial effects compared with the prior art:
according to the invention, plant gum (namely saponin gum powder, sesbania gum powder and guar gum powder) is modified by galactose oxidase and mannose, so that the gluing lag of AKD (alkyl ketene dimer) can be improved, the gluing efficiency of the AKD is improved, and a large amount of cations can be carried in the plant gum through the reaction with 3-chloro, 2-hydroxypropyl trimethyl ammonium chloride and alkali liquor, so that the emulsified AKD emulsion has more positive charges, and the positive charges can be mutually attracted with negative charges in paper pulp fibers in the papermaking gluing process, thereby improving the retention rate of the AKD on the paper fibers; secondly, the polymer emulsified AKD formed by graft polymerization of the acetaldehyde resin and the cation modified plant rubber powder can improve the water resistance of the paper after sizing and can quickly achieve quick curing after sizing, so that the sizing stability of the AKD can be improved, and the performance of the paper processed and produced after the AKD is sized is enhanced.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the process for preparing the AKD emulsion based on the composite cationic vegetable gum polymer comprises the following preparation steps:
s1, adding alkali liquor into a reaction kettle, then adding 28 parts of saponin rubber powder, 25 parts of sesbania gum powder and 35 parts of guar gum powder under the stirring condition of 300rpm, adding galactose oxidase and mannose when the stirring speed is increased to 600rpm, uniformly dispersing, reacting for 3 hours at 120 ℃, pouring the obtained product into an ethanol aqueous solution, adjusting the pH value to 7, filtering out supernate, washing precipitate by using the ethanol aqueous solution, drying and crushing to obtain modified plant rubber powder;
s2, weighing 100 parts of modified plant rubber powder in the S1 into a clean and dry reaction kettle, spraying alkali liquor into the kettle under the condition of stirring, reacting for 25min at 50 ℃, spraying a mixture of an etherifying agent and the alkali liquor, reacting for 3h at 65 ℃, discharging, washing and soaking a discharged product for two times by using 60% ethanol, soaking and washing for 30min by using absolute ethanol, and performing suction filtration and drying to obtain the cationic modified plant rubber powder;
s3, weighing 30 parts of oxidized cation modified plant rubber powder, slowly adding the oxidized cation modified plant rubber powder into a container filled with 60 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant pressure funnel, starting the electric stirrer, adding a self-made acetaldehyde resin solution, heating to 60 ℃, adding 0.3 part of sodium dodecyl sulfate and 1 part of tributyl phosphate, and stirring and emulsifying for 30min;
s4, adding 5 parts of ammonium sulfate and 7 parts of vinyl acetate into the system in the S3, reacting for 30min, heating to 70 ℃, then dropwise adding 18 parts of vinyl acetate again, heating to 80 ℃ after dropwise adding is completed within 3h, keeping the temperature for 30min, then adding 0.2 part of sodium thiosulfate, finally heating to 90 ℃, keeping the temperature for 30min, cooling, discharging, and then regulating the viscosity by using a viscosity stabilizer to obtain the cationic modified vegetable gum-acetaldehyde resin polymer;
s5, weighing 200 parts of AKD and 100 parts of deionized water, adding the AKD and the deionized water into a three-neck flask, stirring, heating to completely melt the AKD and the deionized water at 60 ℃, increasing the rotation speed, adding 25 parts of the S4 cation modified vegetable gum-acetaldehyde resin polymer and 10 parts of the auxiliary emulsifier, premixing for 5min, and transferring the mixture into a homogenizer;
and S6, adding 3 parts of dispersing agent into the system in the homogenizer in S5, uniformly mixing, then, carrying out high-speed shearing emulsification for 10min at the rotating speed of 10000r/min by using a high-shear emulsifying machine, cooling to room temperature, then, adding 13 parts of polyaluminum chloride, and uniformly mixing to obtain the AKD emulsion based on the composite cationic vegetable gum polymer.
The alkali liquor in S1 and S2 is prepared 4% sodium hydroxide solution.
The total mass of the two alkali liquors in the S2 is 30 percent of the total system mass.
The etherifying agent in S2 is 3-chlorine, 2-hydroxypropyl trimethyl ammonium chloride, and the mass of the etherifying agent is 40% of the mass of the total system.
The method for modifying the vegetable gum powder by oxidizing the cations in the S3 comprises the following steps: weighing 50 parts of cation modified plant rubber powder in S2, slowly adding the cation modified plant rubber powder into a container filled with 100 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, then adding 0.1 part of ferrous sulfate at 50 ℃, slowly dropwise adding 3 parts of hydrogen peroxide, oxidizing for 15min, then adding 0.3 part of sodium thiosulfate, standing for 30min, discharging, performing suction filtration by a sand core funnel, washing and drying to obtain the oxidized cation modified plant rubber powder.
The stirring speed was 400r/min, and the dropping speed of the dropwise addition of hydrogen peroxide was 1 drop/s.
The preparation method of the acetaldehyde resin solution in S4 comprises the following steps:
step 1, weighing 20g of polyvinyl alcohol and 150mL of distilled water, adding the polyvinyl alcohol and the distilled water into a three-opening beaker with a spherical condenser tube, a polytetrafluoroethylene electric stirrer and a constant-pressure funnel, standing for 30min, starting the electric stirrer, and preserving heat at 95 ℃ for 30min until the polyvinyl alcohol is completely dissolved;
and 2, cooling the system in the step 1 to 70 ℃, adjusting the pH value to 3 by using a hydrochloric acid solution, dripping 6mL of glyoxal within 30min, keeping the temperature for 1h after dripping is finished, adjusting the pH value to be neutral by using a sodium hydroxide solution, cooling and discharging to obtain the acetaldehyde resin solution.
The mass of the viscosity stabilizer in S4 was 3% of the total system mass, and the viscosity of the cation-modified vegetable gum-acetaldehyde resin polymer in S4 was 2800mPa · S.
The auxiliary emulsifier in S5 is a starch emulsifier.
The dispersant in S6 is hexenyl bis stearamide.
Example 2:
the process for preparing the AKD emulsion based on the composite cationic vegetable gum polymer comprises the following preparation steps:
s1, adding alkali liquor into a reaction kettle, then adding 30 parts of saponin rubber powder, 28 parts of sesbania rubber powder and 40 parts of guar gum powder under the stirring condition of 400rpm, adding galactose oxidase and mannose when the stirring speed is increased to 800rpm, uniformly dispersing, reacting for 4 hours at 130 ℃, pouring the obtained product into an ethanol water solution, adjusting the pH value to 7, filtering out supernate, washing the precipitate with the ethanol water solution, drying and crushing to obtain modified plant rubber powder;
s2, weighing 100 parts of the modified plant rubber powder in the S1 into a clean and dry reaction kettle, spraying alkali liquor into the kettle under the condition of stirring, reacting for 30min at 50 ℃, spraying a mixture of an etherifying agent and the alkali liquor, reacting for 4h at 65 ℃, discharging, washing and soaking a discharged product for two times by using 60% ethanol, then soaking and washing for 30min by using absolute ethanol, and performing suction filtration and drying to obtain the cationic modified plant rubber powder;
s3, weighing 30 parts of oxidized cation modified plant rubber powder, slowly adding the oxidized cation modified plant rubber powder into a container filled with 60 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, starting the electric stirrer, adding a self-made acetaldehyde resin solution, heating to 60 ℃, adding 0.3 part of sodium dodecyl sulfate and 1 part of tributyl phosphate, and stirring and emulsifying for 30min;
s4, adding 8 parts of ammonium sulfate and 8 parts of vinyl acetate into the system in the S3, reacting for 30min, heating to 70 ℃, then dropwise adding 18 parts of vinyl acetate again, heating to 80 ℃ after dropwise adding is completed within 3h, preserving heat for 30min, then adding 0.2 part of sodium thiosulfate, finally heating to 90 ℃, preserving heat for 30min, cooling, discharging, and then using a viscosity stabilizer to adjust viscosity, thus obtaining the cationic modified vegetable gum-acetaldehyde resin polymer;
s5, weighing 200 parts of AKD and 100 parts of deionized water, adding the AKD and the deionized water into a three-neck flask, stirring, heating to completely melt the AKD and the deionized water at 60 ℃, increasing the rotation speed, adding 28 parts of the cation modified vegetable gum-acetaldehyde resin polymer in the S4 and 15 parts of the auxiliary emulsifier, premixing for 5min, and transferring the mixture into a homogenizer;
and S6, adding 5 parts of dispersing agent into the system in the homogenizer in S5, uniformly mixing, then, carrying out high-speed shearing emulsification for 20min at the rotating speed of 10000r/min by using a high-shear emulsifying machine, cooling to room temperature, then, adding 15 parts of polyaluminum chloride, and uniformly mixing to obtain the AKD emulsion based on the composite cationic vegetable gum polymer.
The alkali liquor in S1 and S2 is prepared 4% sodium hydroxide solution.
The total mass of the two alkali liquors in the S2 accounts for 30% of the total mass of the system.
The etherifying agent in S2 is 3-chlorine, 2-hydroxypropyl trimethyl ammonium chloride, and the mass of the etherifying agent is 40% of the mass of the total system.
The method for modifying the plant rubber powder by oxidizing the cations in the S3 comprises the following steps: weighing 50 parts of cation modified plant rubber powder in S2, slowly adding the cation modified plant rubber powder into a container filled with 100 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, then adding 0.1 part of ferrous sulfate at 50 ℃, slowly dropwise adding 3 parts of hydrogen peroxide, oxidizing for 20min, then adding 0.3 part of sodium thiosulfate, standing for 30min, discharging, performing suction filtration by a sand core funnel, washing and drying to obtain the oxidized cation modified plant rubber powder.
The stirring speed was 500r/min, and the dropping speed of dropping hydrogen peroxide was 2 drops/s.
The preparation method of the acetaldehyde resin solution in S4 comprises the following steps:
step 1, weighing 20g of polyvinyl alcohol and 150mL of distilled water, adding the polyvinyl alcohol and the distilled water into a three-opening beaker with a spherical condenser tube, a polytetrafluoroethylene electric stirrer and a constant-pressure funnel, standing for 30min, starting the electric stirrer, and preserving heat at 95 ℃ for 30min until the polyvinyl alcohol is completely dissolved;
and 2, cooling the system in the step 1 to 70 ℃, adjusting the pH value to 4 by using a hydrochloric acid solution, dripping 6mL of glyoxal within 30min, keeping the temperature for 1h after dripping is finished, adjusting the pH value to be neutral by using a sodium hydroxide solution, cooling and discharging to obtain the acetaldehyde resin solution.
The mass of the viscosity stabilizer in S4 was 3% of the total system mass, and the viscosity of the cation-modified vegetable gum-acetaldehyde resin polymer in S4 was 2900mPa · S.
The auxiliary emulsifier in S5 is a starch emulsifier.
The dispersant in S6 is hexenyl bis stearamide.
Example 3:
the process for preparing the AKD emulsion based on the composite cationic vegetable gum polymer comprises the following preparation steps:
s1, adding alkali liquor into a reaction kettle, then adding 29 parts of saponin rubber powder, 26 parts of sesbania rubber powder and 38 parts of guar gum powder under the stirring condition of 300rpm, adding galactose oxidase and mannose when the stirring speed is increased to 700rpm, uniformly dispersing, reacting for 4 hours at 125 ℃, pouring the obtained product into an ethanol water solution, adjusting the pH value to 7, filtering out supernate, washing the precipitate by using the ethanol water solution, drying and crushing to obtain modified plant rubber powder;
s2, weighing 100 parts of the modified plant rubber powder in the S1 into a clean and dry reaction kettle, spraying alkali liquor into the kettle under the condition of stirring, reacting for 28min at 50 ℃, spraying a mixture of an etherifying agent and the alkali liquor, reacting for 3h at 65 ℃, discharging, washing and soaking a discharged product for two times by using 60% ethanol, then soaking and washing for 30min by using absolute ethanol, and performing suction filtration and drying to obtain the cationic modified plant rubber powder;
s3, weighing 30 parts of oxidized cation modified plant rubber powder, slowly adding the oxidized cation modified plant rubber powder into a container filled with 60 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, starting the electric stirrer, adding a self-made acetaldehyde resin solution, heating to 60 ℃, adding 0.3 part of sodium dodecyl sulfate and 1 part of tributyl phosphate, and stirring and emulsifying for 30min;
s4, adding 7 parts of ammonium sulfate and 8 parts of vinyl acetate into the system in the S3, reacting for 30min, heating to 70 ℃, then dropwise adding 18 parts of vinyl acetate again, heating to 80 ℃ after dropwise adding is completed within 3h, preserving heat for 30min, then adding 0.2 part of sodium thiosulfate, finally heating to 90 ℃, preserving heat for 30min, cooling, discharging, and then using a viscosity stabilizer to adjust viscosity, thus obtaining the cationic modified vegetable gum-acetaldehyde resin polymer;
s5, weighing 200 parts of AKD and 100 parts of deionized water, adding the AKD and the deionized water into a three-neck flask, stirring, heating to completely melt the AKD and the deionized water at 60 ℃, increasing the rotation speed, adding 26 parts of the S4 cation modified vegetable gum-acetaldehyde resin polymer and 13 parts of the auxiliary emulsifier, premixing for 5min, and transferring the mixture into a homogenizer;
and S6, adding 4 parts of dispersing agent into the system in the homogenizer in S5, uniformly mixing, performing high-speed shearing emulsification for 15min at the rotating speed of 10000r/min by using a high-shear emulsifying machine, cooling to room temperature, adding 14 parts of polyaluminum chloride, and uniformly mixing to obtain the AKD emulsion based on the composite cationic vegetable gum polymer.
The alkali liquor in S1 and S2 is prepared 4% sodium hydroxide solution.
The total mass of the two alkali liquors in the S2 accounts for 30% of the total mass of the system.
The etherifying agent in S2 is 3-chlorine, 2-hydroxypropyl trimethyl ammonium chloride, and the mass of the etherifying agent is 40% of the mass of the total system.
The method for modifying the vegetable gum powder by oxidizing the cations in the S3 comprises the following steps: weighing 50 parts of cation modified plant rubber powder in S2, slowly adding the cation modified plant rubber powder into a container filled with 100 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, then adding 0.1 part of ferrous sulfate at 50 ℃, slowly dropwise adding 3 parts of hydrogen peroxide, oxidizing for 18min, then adding 0.3 part of sodium thiosulfate, standing for 30min, discharging, performing suction filtration by a sand core funnel, washing and drying to obtain the oxidized cation modified plant rubber powder.
The stirring speed was 400r/min, and the dropping speed of dropping hydrogen peroxide was 2 drops/s.
The preparation method of the acetaldehyde resin solution in S4 comprises the following steps:
step 1, weighing 20g of polyvinyl alcohol and 150mL of distilled water, adding the polyvinyl alcohol and the distilled water into a three-opening beaker with a spherical condenser tube, a polytetrafluoroethylene electric stirrer and a constant-pressure funnel, standing for 30min, starting the electric stirrer, and preserving heat at 95 ℃ for 30min until the polyvinyl alcohol is completely dissolved;
and 2, cooling the system in the step 1 to 70 ℃, adjusting the pH value to 4 by using a hydrochloric acid solution, dripping 6mL of glyoxal within 30min, keeping the temperature for 1h after dripping is finished, adjusting the pH value to be neutral by using a sodium hydroxide solution, cooling and discharging to obtain the acetaldehyde resin solution.
The mass of the viscosity stabilizer in S4 was 3% of the total system mass, and the viscosity of the cation-modified vegetable gum-acetaldehyde resin polymer in S4 was 2800mPa · S.
The auxiliary emulsifier in S5 is a starch emulsifier.
The dispersant in S6 is hexenyl bis stearamide.
Performance testing
1. The AKD emulsions prepared in examples 1 to 3 based on complex cationic vegetable gum polymers were respectively labeled as examples 1, 2 and 3, the AKD emulsions prepared by emulsifying a common emulsifier on the market were labeled as comparative examples, and the performances of examples 1, 2, 3 and comparative examples were tested and reported as follows:
2. the papers produced after sizing the AKD emulsions based on complex cationic vegetable gum polymers prepared in examples 1-3 were labeled as examples 1, 2, 3, respectively, and the papers produced after sizing the AKD emulsions prepared by emulsifying a common emulsifier on the market were labeled as comparative examples, and the performance of examples 1, 2, 3 and comparative examples were tested and reported as follows:
the data in the table show that the stability and dispersibility of the AKD emulsion based on the composite cationic vegetable gum polymer prepared in the embodiments 1-3 of the present invention are higher than those of the AKD emulsion prepared by emulsifying with a common emulsifying agent in the market, and the performance of the paper produced by sizing the AKD emulsion based on the composite cationic vegetable gum polymer prepared in the embodiments 1-3 of the present invention is higher than that of the paper produced by sizing the AKD emulsion prepared by emulsifying with a common emulsifying agent, so that the process for preparing the AKD emulsion based on the composite cationic vegetable gum polymer designed by the present invention has excellent market popularization value.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a," "8230," "8230," or "comprising" does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A process for preparing AKD emulsion based on composite cationic vegetable gum polymer is characterized by comprising the following preparation steps:
s1, adding alkali liquor into a reaction kettle, then adding 28-30 parts of saponin rubber powder, 25-28 parts of sesbania rubber powder and 35-40 parts of guar gum powder under the stirring condition of 300-400rpm, adding galactose oxidase and mannose enzyme when the stirring speed is increased to 600-800rpm, reacting for 3-4 hours at 120-130 ℃ after uniform dispersion, pouring the obtained product into an ethanol water solution to adjust the pH value to 7, filtering out supernate, washing precipitate by using the ethanol water solution, drying and crushing to obtain modified plant rubber powder;
s2, weighing 100 parts of modified plant gum powder in S1, putting the modified plant gum powder into a clean and dry reaction kettle, spraying alkali liquor into the kettle under the condition of stirring, reacting for 25-30min at 50 ℃, spraying a mixture of an etherifying agent and the alkali liquor, reacting for 3-4h at 65 ℃, discharging, washing and soaking a discharged product for two times by using 60% ethanol, soaking and washing for 30min by using absolute ethanol, and performing suction filtration and drying to obtain the cationic modified plant gum powder;
s3, weighing 30 parts of oxidized cation modified plant rubber powder, slowly adding the oxidized cation modified plant rubber powder into a container filled with 60 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant-pressure funnel, starting the electric stirrer, adding a self-made acetaldehyde resin solution, heating to 60 ℃, adding 0.3 part of sodium dodecyl sulfate and 1 part of tributyl phosphate, and stirring and emulsifying for 30min;
s4, adding 5-8 parts of ammonium sulfate and 7-8 parts of vinyl acetate into the system in the S3, reacting for 30min, heating to 70 ℃, then dropwise adding 18 parts of vinyl acetate again, after dropwise adding is completed within 3h, heating to 80 ℃, preserving heat for 30min, then adding 0.2 part of sodium thiosulfate, finally heating to 90 ℃, preserving heat for 30min, cooling, discharging, and then using a viscosity stabilizer to adjust viscosity, thus obtaining the cationic modified vegetable gum-acetaldehyde resin polymer;
s5, weighing 200 parts of AKD and 100 parts of deionized water, adding the AKD and the deionized water into a three-neck flask, stirring, heating to completely melt the AKD and the deionized water at 60 ℃, increasing the rotation speed, adding 25-28 parts of the cation modified vegetable gum-acetaldehyde resin polymer in S4 and 10-15 parts of the auxiliary emulsifier, premixing for 5min, and transferring the mixture into a homogenizer;
and S6, adding 3-5 parts of dispersing agent into a system in a homogenizer in S5, uniformly mixing, performing high-speed shearing emulsification for 10-20min at a rotating speed of 10000r/min by using a high-shear emulsifying machine, cooling to room temperature, adding 13-15 parts of polyaluminum chloride, and uniformly mixing to obtain the AKD emulsion based on the composite cationic vegetable gum polymer.
2. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 1, wherein the alkali solution in S1 and S2 is prepared 4% sodium hydroxide solution.
3. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 1, wherein the total mass of the two alkali solutions in S2 is 30% of the mass of the total system.
4. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 1, wherein the etherifying agent in S2 is 3-chloro, 2-hydroxypropyl trimethyl ammonium chloride, and the mass of etherifying agent is 40% of the total system mass.
5. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 1, wherein the method for oxidizing cationic modified vegetable gum powder in S3 comprises: weighing 50 parts of cation modified plant rubber powder in S2, slowly adding the cation modified plant rubber powder into a container filled with 100 parts of distilled water, uniformly stirring, adding the system into a four-neck flask provided with a polytetrafluoroethylene electric stirrer, a spherical reflux condenser tube and a constant pressure funnel, then adding 0.1 part of ferrous sulfate at 50 ℃, slowly dropwise adding 3 parts of hydrogen peroxide, oxidizing for 15-20min, then adding 0.3 part of sodium thiosulfate, standing for 30min, discharging, performing suction filtration by a sand core funnel, washing and drying to obtain the oxidized cation modified plant rubber powder.
6. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 5, wherein the stirring speed is 400-500r/min, and the dropping speed of dropping hydrogen peroxide is 1-2 drops/s.
7. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 1, wherein the preparation method of the acetaldehyde resin solution in S4 comprises the following steps:
step 1, weighing 20g of polyvinyl alcohol and 150mL of distilled water, adding the polyvinyl alcohol and the distilled water into a three-opening beaker with a spherical condenser tube, a polytetrafluoroethylene electric stirrer and a constant-pressure funnel, standing for 30min, starting the electric stirrer, and preserving heat at 95 ℃ for 30min until the polyvinyl alcohol is completely dissolved;
and 2, cooling the system in the step 1 to 70 ℃, adjusting the pH to 3-4 by using a hydrochloric acid solution, dripping 6mL of glyoxal within 30min, keeping the temperature for 1h after dripping is finished, adjusting the pH to be neutral by using a sodium hydroxide solution, cooling and discharging to obtain the acetaldehyde resin solution.
8. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer according to claim 1, wherein the mass of the viscosity stabilizer in S4 is 3% of the total system mass, and the viscosity of the cationic modified vegetable gum-acetaldehyde resin polymer in S4 is 2800-2900 mPa-S.
9. The process for preparing AKD emulsion based on complex cationic vegetable gum polymer as claimed in claim 1, wherein the co-emulsifier in S5 is starch emulsifier.
10. The process for preparing AKD emulsion based on composite cationic vegetable gum polymer as claimed in claim 1, wherein the dispersant in S6 is hexenyl bis stearamide.
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