CN112878097B - Preparation method of alkyl ketene dimer papermaking sizing agent and product - Google Patents
Preparation method of alkyl ketene dimer papermaking sizing agent and product Download PDFInfo
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- CN112878097B CN112878097B CN202110033769.3A CN202110033769A CN112878097B CN 112878097 B CN112878097 B CN 112878097B CN 202110033769 A CN202110033769 A CN 202110033769A CN 112878097 B CN112878097 B CN 112878097B
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- 238000004513 sizing Methods 0.000 title claims abstract description 69
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- -1 alkyl ketene dimer Chemical compound 0.000 title claims abstract description 18
- 239000000839 emulsion Substances 0.000 claims abstract description 64
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000011259 mixed solution Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 229910000271 hectorite Inorganic materials 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004945 emulsification Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 9
- 229960004624 perflexane Drugs 0.000 claims abstract description 9
- ZJIJAJXFLBMLCK-UHFFFAOYSA-N perfluorohexane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F ZJIJAJXFLBMLCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 9
- YVBBRRALBYAZBM-UHFFFAOYSA-N perfluorooctane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YVBBRRALBYAZBM-UHFFFAOYSA-N 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 229940045860 white wax Drugs 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003995 emulsifying agent Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 14
- 230000001804 emulsifying effect Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 7
- 239000004094 surface-active agent Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229940014800 succinic anhydride Drugs 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 2
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 2
- 235000013922 glutamic acid Nutrition 0.000 description 2
- 239000004220 glutamic acid Substances 0.000 description 2
- 229960001545 hydrotalcite Drugs 0.000 description 2
- 229910001701 hydrotalcite Inorganic materials 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 150000002596 lactones Chemical class 0.000 description 2
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 2
- 239000008108 microcrystalline cellulose Substances 0.000 description 2
- 229940016286 microcrystalline cellulose Drugs 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229920001661 Chitosan Polymers 0.000 description 1
- 241000212749 Zesius chrysomallus Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 238000009924 canning Methods 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
Images
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
- 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
- D21H17/17—Ketenes, e.g. ketene dimers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/64—Paper recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
Abstract
The invention provides a preparation method of an alkyl ketene dimer papermaking sizing agent, which comprises the following steps: mixing the hectorite aqueous dispersion with acetone, ammonia monohydrate and hexadecyl trimethyl siloxane, and performing ultrasonic dispersion to obtain a mixed solution I; adding tridecafluorooctyltriethoxysilane into the mixed solution I, and performing ultrasonic dispersion to obtain a mixed solution II; drying the mixed solution II to obtain modified hectorite powder; mixing the modified hectorite powder with perfluorohexane, performing ultrasonic dispersion, adding molten AKD, mixing, heating, and performing ultrasonic emulsification to obtain AKD-A emulsion; and mixing the AKD-A emulsion with a sodium dodecyl sulfate aqueous solution, and performing ultrasonic emulsification to obtain the alkyl ketene dimer papermaking sizing agent. The AKD emulsion prepared by the method has obviously improved sizing performance, and can greatly improve the hydrolysis resistance and emulsion stability of the AKD; the AKD sizing agent emulsion has the advantages of simple preparation process, small using amount of the emulsifier, low emulsification cost and good sizing effect.
Description
Technical Field
The invention relates to the technical field of papermaking, in particular to a preparation method of an alkyl ketene dimer papermaking sizing agent emulsion and a product.
Background
The paper making industry in the twentieth century changes from an acidic paper making system to a medium-alkaline paper making system, is an innovative change of a paper making process, greatly improves the paper quality, expands the filler range, reduces the pulp consumption and the energy consumption, lightens the environmental pollution, and prolongs the service life of equipment. According to data statistics, the cultural paper produced by the medium and alkaline sizing accounts for 60-65% of the total amount of the cultural paper in the beginning of the 80 th year in Europe, the cultural paper reaches 95% in the 90 th year, and the medium and alkaline sizing proportion of the high-grade paper in the United states at the same time is increased from 15% to more than 90%. Since 1989, the use of medium-and alkaline sizing in production has begun, and the application thereof has gradually become popular in recent years, and Alkyl Ketene Dimer (AKD) and Alkenyl Succinic Anhydride (ASA) are mainly used at present.
AKD is unsaturated lactone, is water-insoluble waxy solid at normal temperature, can be used as a papermaking sizing agent, but must be prepared into emulsion before use, and is one of sizing agents commonly used for alkaline sizing in the current papermaking industry. The other commonly used papermaking sizing agent alkenyl succinic anhydride is liquid at normal temperature, the anhydride in the molecular structure is very easy to hydrolyze, the storage stability is poor, workshop on-site emulsification is needed, and the hydrolysis product is easy to deposit on a paper machine to cause papermaking obstacle, so the application of the alkenyl succinic anhydride is limited to a certain extent. The lactone ring in the AKD emulsion has low hydrolysis speed, emulsion drops are solid particles at normal temperature, the emulsion has good storage property, the emulsion prepared by the good emulsification process can be placed for 2-3 months, the sizing efficiency is high, the cost is relatively low, and the advantages promote the wide application of the AKD emulsion. However, compared with alkenyl succinic anhydride, AKD emulsion has storage requirement, and the emulsion is required to have long-term emulsion droplet aggregation resistance and other properties, and the emulsification process requirement is more severe. The AKD emulsifying process is generally heating to melt, then adding dispersant, surfactant, gelatinized cationic starch and the like, homogenizing and emulsifying after premixing, cooling and canning after homogenizing. The surfactant added in the emulsification process can reduce the sizing efficiency, easily generate air bubbles, bring the foaming problem to a paper making system and even generate paper defects. Therefore, the development of an efficient AKD emulsifying system and the reduction of the dosage of the surfactant even without the surfactant are beneficial to improving the AKD sizing efficiency, and the AKD sizing agent is suitable for the production requirements of paper-making enterprises and the requirements of the current green production.
Patent publication No. CN 104499361 discloses a preparation method of AKD sizing agent of nano microcrystalline cellulose, which avoids the use of surface sizing agent, can be used for both surface sizing and internal sizing of paper pulp, and obviously improves the sizing degree of paper industry, but the existing preparation method of microcrystalline cellulose is more complex and expensive, and is not beneficial to wide industrial application. Patent publication No. CN 103774496 discloses an AKD emulsion stabilized by glutamic acid, hydrotalcite and poly diallyl dimethyl ammonium chloride, and the publication patent mentions that the AKD emulsion stabilized by glutamic acid and hydrotalcite alone is unstable, the emulsion formed by adding poly diallyl dimethyl ammonium chloride has good stability and sizing performance, and a cationic surfactant (poly diallyl dimethyl ammonium chloride) is still used in the emulsion preparation process. Chinese patent 201010281410.X discloses a method for jointly emulsifying AKD by chitosan and nano titanium dioxide, which has the advantages of simple emulsifying process, high AKD emulsion sizing efficiency and high curing speed, but emulsion drop coalescence stability is still to be improved. In view of the wide use of AKD and the problems existing at present, a new AKD emulsion preparation technology needs to be further researched to prepare sizing agents which have high sizing efficiency and are suitable for modern paper making enterprises.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the AKD sizing agent emulsion with higher stability and sizing activity.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of an alkyl ketene dimer papermaking sizing agent comprises the following steps:
(1) mixing the hectorite aqueous dispersion with acetone, ammonia monohydrate and hexadecyl trimethyl siloxane, and performing ultrasonic dispersion to obtain a mixed solution I; adding tridecafluorooctyltriethoxysilane into the mixed solution I, and performing ultrasonic dispersion to obtain a mixed solution II; drying the mixed solution II to obtain modified hectorite powder;
(2) mixing the modified hectorite powder with perfluorohexane, performing ultrasonic dispersion, adding molten AKD, mixing, heating, and performing ultrasonic emulsification to obtain AKD-A emulsion;
(3) and mixing the AKD-A emulsion with a sodium dodecyl sulfate aqueous solution, and performing ultrasonic emulsification to obtain the AKD-B emulsion, namely the papermaking sizing agent.
The hectorite is original flake-shaped nano particles, the diameter of the hectorite is 25-100nm, and the thickness of the hectorite is 2-10 nm.
The mass fraction of the hectorite in the mixed solution I is 0.05-2%, the mass fraction of the acetone is 0.1-1%, and the mass fraction of the ammonium monohydrate is 0.5-2%.
The dosage of the hexadecyl trimethyl siloxane is 2-30% of the mass of the hectorite.
The dosage of the tridecafluorooctyltriethoxysilane accounts for 5-20% of the mass of the hectorite.
The AKD is white wax flake solid alkyl ketene dimer at normal temperature, and the AKD in a molten state is liquid AKD with good flow at 85 ℃.
In the step (2), the heating temperature is 85 ℃.
The mass ratio of the modified hectorite powder to the perfluorooctane is 1: 20-100.
The mass ratio of the AKD to the perfluorooctane is 1: 0.1-2.
The mass ratio of the AKD-A emulsion to the sodium dodecyl sulfate aqueous solution is 1: 0.5-10.
The mass percentage of the sodium dodecyl sulfate aqueous solution is 0.1-2%, preferably 0.2-1%.
The power of the ultrasonic dispersion is 500-3000W.
An alkyl ketene dimer papermaking sizing agent obtained by the preparation method.
An application of the alkyl ketene dimer papermaking sizing agent in preparing paper.
The invention has the following advantages:
the invention respectively modifies the hectorite by hexadecyl trimethyl siloxane and tridecafluorooctyl triethoxysilane, and introduces a group of a hydrocarbon-philic oil phase and a group of a fluorocarbon-philic oil phase; and the oil-in-water-in-oil (W/O/O) type composite AKD emulsion emulsified and stabilized by utilizing the modified nano-scale hectorite and the sodium dodecyl sulfate has ultrahigh stability and strong hydrolysis resistance. The AKD sizing agent emulsion prepared by the invention can not generate particle aggregation and precipitation after being placed for 180 days, has no phase body precipitation and no demulsification phenomenon, has good emulsion stability, almost has no attenuation on the sizing degree of sized paper, can reach 765 seconds when the internal sizing dosage of paper pulp is 0.2 percent (relative to the mass percent of absolutely dry pulp), and has good sizing performance and hydrolysis resistance. Compared with the traditional AKD emulsion with stable emulsification of a surfactant (such as starch) and the AKD emulsion with stable emulsification of solid particles (such as clay nanoparticles and modified particles thereof), the AKD emulsion prepared by the method has the advantages that the sizing performance is remarkably improved, and meanwhile, the hydrolysis resistance and the emulsion stability of the AKD can be greatly improved; the AKD sizing agent emulsion has the advantages of simple preparation process, small using amount of the emulsifying agent, low emulsifying cost and good sizing effect.
Drawings
FIG. 1 is a micrograph of AKD-A emulsion prepared in example 2;
FIG. 2 is a micrograph of AKD-B emulsion prepared in example 2;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the AKD-B emulsion prepared in example 2.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited to the following examples.
Example 1 preparation of AKD sizing agent
(1) 1 part by weight of hectorite (the average width of a single particle is 25nm, the thickness is 2 nm) is dispersed in water to prepare a dispersion liquid with the mass fraction of 0.05 percent, 2 parts by weight of acetone, 10 parts by weight of ammonium monohydrate and 0.02 part by weight of hexadecyl trimethyl siloxane are added and mixed, and the mixture is ultrasonically dispersed for 1 hour at the temperature of 25 ℃ under the condition of 500W to obtain a mixed solution I; adding 0.05 part by weight of tridecafluorooctyltriethoxysilane into the mixed solution I, and continuing to perform ultrasonic dispersion for 1 hour to obtain mixed solution II; vacuum drying the mixed solution II at 65 ℃ to obtain modified hectorite powder;
(2) mixing 1 part by weight of modified hectorite powder with 20 parts by weight of perfluorohexane, ultrasonically dispersing at 25 ℃ for 1 hour by 500W, adding 200 parts by weight of molten AKD, mixing, continuously ultrasonically emulsifying at 85 ℃ for 15 minutes, and cooling to room temperature to obtain AKD-A emulsion;
(3) mixing 2 parts by weight of AKD-A emulsion with 1 part by weight of sodium dodecyl sulfate aqueous solution with the mass concentration of 0.1%, and ultrasonically emulsifying for 15 minutes at the temperature of 25 ℃ at 500W to obtain AKD-B emulsion, namely the AKD sizing agent.
Example 2 preparation of AKD sizing agent
(1) 1 part by weight of hectorite (the average width of a single particle is 38nm and the thickness is 6 nm) is dispersed in water to prepare a dispersion liquid with the mass fraction of 1 percent, 10 parts by weight of acetone, 20 parts by weight of ammonium monohydrate and 0.2 part by weight of hexadecyl trimethyl siloxane are added and mixed, and ultrasonic dispersion is carried out for 1 hour at 1000W at 25 ℃ to obtain a mixed solution I; adding 0.1 part by weight of tridecafluorooctyltriethoxysilane into the mixed solution I, and continuing to perform ultrasonic dispersion for 1 hour to obtain mixed solution II; vacuum drying the mixed solution II at 65 ℃ to obtain modified hectorite powder;
(2) mixing 1 part by weight of modified hectorite powder with 60 parts by weight of perfluorohexane, performing ultrasonic dispersion at 25 ℃ for 1 hour at 1000W, adding 60 parts by weight of molten AKD, mixing, and performing ultrasonic emulsification at 85 ℃ for 15 minutes to obtain AKD-A emulsion; the micrograph is shown in figure 1: wherein the continuous phase is perfluorohexane, the droplets are AKD emulsion (oil-in-oil) droplets coated with perfluorohexane, and the interface component of the droplets is grafted with long-chain alkyl group [ - (CH) 2 ) x CH 3 ]And long-chain perfluoroalkane group [ - (CH) 2 ) x (CF 2 ) x CF 3 ]Modified hectorite particles effective as interfacial particle stabilizers to stabilize perfluorohexane and AKD oil phases to form AKD-A emulsions having an average droplet diameter of about 5 μm;
(3) mixing 1 part by weight of AKD-A emulsion with 5 parts by weight of sodium dodecyl sulfate aqueous solution with the mass concentration of 0.5%, and ultrasonically emulsifying for 15 minutes at the temperature of 25 ℃ under 1000W to obtain AKD-B emulsion, namely the AKD sizing agent, wherein a micrograph of the AKD-B emulsion is shown in figure 2, and an SEM picture is shown in figure 3: the sizing agent emulsion takes sodium dodecyl sulfate aqueous solution as a continuous phase, and the AKD-perfluorooctane emulsion is uniformly dispersed in the aqueous solution in a spherical dispersion liquid drop form; wherein AKD is coated by perfluorooctane, and the modified hectorite is adsorbed at an oil-oil interface between the AKD and the perfluorooctane in the form of solid particles to form an oil-oil emulsion; the AKD emulsion liquid drop obtained finally avoids the contact with a water phase due to the wrapping of the outer oil phase, thereby achieving the purpose of avoiding hydrolysis.
Example 3 preparation of AKD sizing agent
(1) Dispersing 2 parts by weight of hectorite (the average width of a single particle is 50nm, and the thickness of the single particle is 10 nm) in water to prepare a dispersion liquid with the mass fraction of 2%, adding 1 part by weight of acetone, 2 parts by weight of ammonium monohydrate and 0.6 part by weight of hexadecyl trimethyl siloxane, mixing, and performing ultrasonic dispersion at the temperature of 25 ℃ under 3000W for 1 hour to obtain a mixed solution I; adding 0.4 part by weight of tridecafluorooctyltriethoxysilane into the mixed solution I, and continuing to perform ultrasonic dispersion for 1 hour to obtain mixed solution II; vacuum drying the mixed solution II at 65 ℃ to obtain modified hectorite powder;
(2) mixing 1 part by weight of modified hectorite powder with 100 parts by weight of perfluorohexane, ultrasonically dispersing at 3000W at 25 ℃ for 1 hour, adding 10 parts by weight of molten AKD, mixing, and continuously ultrasonically emulsifying at 85 ℃ for 15 minutes to obtain AKD-A emulsion;
(3) mixing 1 part by weight of AKD-A emulsion with 10 parts by weight of 1% sodium dodecyl sulfate aqueous solution, and ultrasonically emulsifying at 25 ℃ for 15 minutes at 3000W to obtain AKD-B emulsion, namely the AKD sizing agent.
Comparative example 1
The AKD sizing agent was prepared according to CN 201810380690.6 a method for preparing AKD paper sizing agent and the product thereof as described in example 3.
Application example AKD sizing agent Performance determination
(1) Paper making of sized paper
Sizing by an internal sizing method. Before sizing, the AKD sizing agents prepared in examples and comparative examples were diluted to 0.5%, the pulp concentration was adjusted to 1%, 1% aluminum sulfate (mass% with respect to the oven-dried pulp) was added to the pulp at a stirring rate of 1000rpm, then the pH of the pulp was adjusted to 7.5 to 8.5 with 1 mol/L sodium hydroxide solution, and then the sizing agent (amount of 0.1%, mass% with respect to the total mass of the oven-dried pulp) and the cationic polyacrylamide (amount of 0.03% (mass% with respect to the oven-dried pulp) were added in this order, and after stirring at a shearing rate of 500rpm for 2 minutes with a stirrer, they were left to stand for 30 seconds, and thenHandsheets were produced with a PTI sheet former (model No. RK3 AKWT) at a basis weight of 60 g/m 2 (T205 om-88, TAPPI), the sheet making system selects a Kaiser method manual sheet making mode to make sheets according to the ISO5289/2 and DIN54358 standards. The handsheets produced by the process are dried at 105 ℃ and then the moisture of the paper is balanced for 24 hours at room temperature, and the ambient humidity is 50%.
(2) Sizing degree measuring method
Sizing performance was evaluated by measuring the degree of sizing of paper made (GB/T5405-2002). Before measurement, the paper was cut into square pieces of 30X 30mm and allowed to stand at 25 ℃ under a 50% humidity environment to equilibrate the moisture for 24 hours. The paper is folded at four sides to form a boat-shaped structure with the bottom surface area of about 20 multiplied by 20mm, then the boat-shaped structure floats in ammonium thiocyanate dilute solution with the concentration of 2 percent, 0.5 mu L of ferric chloride solution with the mass concentration of 1 percent is dripped on the upper part of the boat-shaped paper by a rubber head dropper, and the timing is ended by a stopwatch when red spots appear in the middle of the ferric chloride solution, and the timing is the sizing degree of the paper sample. The front and back sides of the test sample were measured 10 times each and the average was taken.
(3) Method for measuring average particle diameter of liquid drop
The diameters of 100 emulsion droplets observed under a microscope are counted by using particle size counting software carried by an optical microscope, and the average value is taken, namely the average particle size of the droplets.
TABLE 1 Properties of different sizing agents
According to data in table 1, the average diameter of the droplets of the AKD sizing agent emulsion prepared by the invention is smaller, and the emulsion is free from phase body precipitation and demulsification after being placed for 180 days, which indicates that the emulsion has good stability; the paper sheet sizing degree of the sized paper is 734-; the sizing degree of the sizing paper after the emulsion is placed for 180 days is 722 and 785 seconds, which shows that the emulsion has good hydrolysis resistance.
Claims (8)
1. The preparation method of the alkyl ketene dimer papermaking sizing agent is characterized by comprising the following steps:
(1) mixing the hectorite water dispersion with acetone, ammonium monohydrate and hexadecyl trimethyl siloxane, and performing ultrasonic dispersion to obtain a mixed solution I; adding tridecafluorooctyltriethoxysilane into the mixed solution I, and performing ultrasonic dispersion to obtain a mixed solution II; drying the mixed solution II to obtain modified hectorite powder;
(2) mixing the modified hectorite powder with perfluorohexane, performing ultrasonic dispersion, adding molten AKD, mixing, heating, and performing ultrasonic emulsification to obtain AKD-A emulsion;
(3) mixing the AKD-A emulsion with a sodium dodecyl sulfate aqueous solution, and performing ultrasonic emulsification to obtain AKD-B emulsion, namely a papermaking sizing agent;
the dosage of the hexadecyl trimethyl siloxane is 2-30% of the mass of the hectorite; the dosage of the tridecafluorooctyltriethoxysilane accounts for 5 to 20 percent of the mass of the hectorite;
the mass ratio of the modified hectorite powder to the perfluorooctane is 1: 20-100; the mass ratio of the AKD to the perfluorooctane is 1: 0.1-2.
2. The method of claim 1, wherein the hectorite is in the form of raw plate-like nanoparticles having a diameter of 25-100nm and a thickness of 2-10 nm.
3. The preparation method according to claim 1, wherein the mass fraction of hectorite in the mixed solution I is 0.05-2%; the mass fraction of acetone is 0.1-1%; the mass fraction of the ammonia monohydrate is 0.5-2%.
4. The method according to claim 1, wherein the AKD is a white wax sheet-like solid alkyl ketene dimer at normal temperature, and the AKD in a molten state is a liquid AKD that flows well at 85 ℃; in the step (2), the heating temperature is 85 ℃.
5. The preparation method according to claim 1, wherein the mass ratio of the AKD-A emulsion to the aqueous solution of sodium dodecyl sulfate is 1: 0.5-10; the mass percentage of the sodium dodecyl sulfate aqueous solution is 0.1-2%.
6. The preparation method according to claim 1, wherein the power of the ultrasonic dispersion is 500-3000W.
7. An alkyl ketene dimer papermaking sizing agent obtained by the preparation method according to any one of claims 1 to 6.
8. Use of an alkyl ketene dimer papermaking sizing agent as defined in claim 7 in the preparation of paper.
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