CN101338058A - Method for preparing AKD high molecular dispersing agent and use thereof - Google Patents
Method for preparing AKD high molecular dispersing agent and use thereof Download PDFInfo
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Abstract
The invention provides a preparation method for AKD polymeric dispersants and an application thereof. Part of soft monomers, hard monomers, cationic monomers and molecular weight regulators are added into the mixed system of de-ionized water, acid, catalysts and high molecular polymer, initiators are added into the mixture after the temperature is raised, then the temperature is raised to the set value, the rest of soft and hard monomers, cationic monomers, molecular weight regulators and initiators are added, and the mixture reacts for 2 hours to 3 hours under the preserved temperature of 80 DEG C to 85 DEG C and then is cooled to obtain the polymeric dispersants; molten AKD sumatriptan is added into the mixed system of the AKD polymeric dispersant and de-ionized water to be heated up and stirred, and the is homogenized for one time to dilute and obtain cationic AKD latex. The AKD polymeric dispersant has excellent dispersion and emulsification properties; the cationic products obtained by dispersing AKD has high solid content, high electric charge density, small diameters and uniform distribution of the granules, long storage time, excellent surface sizability, fast off-machine slaking, simple synthesis process and low energy consumption.
Description
Technical field
The invention belongs to the papermaking chemical product field, be specifically related to a kind of preparation method and application of AKD macromolecule dispersing agent.
Background technology
Alkyl ketene dimer (AKD) is a kind of reactive sizing agent, and at home and abroad paper industry is used widely in recent years.Since U.S. Hercules company releases cationic AKD emulsion sizing agent first the beginning of the eighties, though still there is solid content low (solid content of product is usually between 12.5%～17%) in product through repeatedly improving, the preparation process complexity, energy consumption is higher (to need 3000 rev/mins of following high speed shear 30min, homogeneous secondary under 26～30Mpa high pressure), following machine slaking slow (generally descend machine 24h after could complete slaking), electric density is low to be difficult for keeping fast on fiber (be lower than+30mv), period of storage short (being less than 2 months), being directly used in problem such as top sizing weak effect is difficult to solve.
The AKD emulsion is a dispersion agent with cationic starch and naphthalene sulfonic acidformaldehyde condensation product tensio-active agent normally at present, by high speed shear and secondary high-pressure homogeneous, advances to dilute the still dilution then and obtains finished product.Other has report to adopt chitosan, hemicellulose and guar gum cation graft polymkeric substance to make AKD dispersion agent preparing product (CN101173026), but its preparation process is added tensio-active agent equally, descends owing to its wetting ability causes the product sizing efficiency by force.Aforesaid method makes that the dispersion agent that contains natural polymer is perishable, period of storage is shorter.
Summary of the invention
The objective of the invention is to solve the shortcoming and defect of above-mentioned currently available products technology, a kind of preparation method of AKD macromolecule dispersing agent is provided and uses the method that this dispersion agent is produced a kind of cation AKD emulsion.
The preparation method of this AKD macromolecule dispersing agent, the raw material that adopts is: acid, catalyzer, high molecular polymer, soft monomer, hard monomer, cationic monomer, molecular weight regulator and initiator, adopt to react in the solution that soft monomer, hard monomer, cationic monomer and molecular weight regulator and initiator adding deionized water, acid, catalyzer and high molecular polymer are mixed to make; And required soft monomer, hard monomer, cationic monomer and molecular weight regulator and the initiator of the preparation method of this AKD macromolecule dispersing agent adds at twice; This preparation method comprises step:
1) deionized water, acid, catalyzer and high molecular polymer are mixed, it is even to be stirred well to system;
2) under whipped state in the liquid in step 1, add part soft monomer, hard monomer, cationic monomer and molecular weight regulator, system heat temperature raising to 73～75 ℃ add the part initiator then, behind insulation 13～17min, are warming up to 76～80 ℃;
3) in step 2 reaction system, drip soft monomer, hard monomer, cationic monomer, molecular weight regulator and the remainder initiator of remainder, wherein soft monomer, hard monomer, cationic monomer and molecular weight regulator dropping time are controlled at 2～3h, and the initiator dropping time is controlled at 2.5～3h;
4) dropwise, again temperature is risen to 80～85 ℃ of following insulation reaction 2～3h, be cooled to room temperature, filter and promptly obtain product; By production requirement, can adopt 200 order nets to filter during filtration;
Wherein, soft monomer in the step 2, hard monomer, the add-on of cationic monomer and molecular weight regulator is respectively soft monomer in the preparation of AKD macromolecule dispersing agent, hard monomer, cationic monomer and molecular weight regulator always add 10%～50% of weight separately, be that the add-on of soft monomer in step 2 always adds 10%～50% of weight for soft monomer in the preparation of AKD macromolecule dispersing agent, the add-on of hard monomer in step 2 always adds 10%～50% of weight for hard monomer in the preparation of AKD macromolecule dispersing agent, the add-on of cationic monomer in step 2 always adds 10%～50% of weight for cationic monomer in the preparation of AKD macromolecule dispersing agent, the add-on of molecular weight regulator in step 2 always adds 10%～50% of weight for molecular weight regulator in the AKD macromolecule dispersing agent preparation, the add-on of initiator then be in the preparation of AKD macromolecule dispersing agent total initiator adding weight 20%～50%; The soft monomer that adds remainder in the step 3, hard monomer, the amount of cationic monomer and molecular weight regulator is soft monomer in the preparation of AKD macromolecule dispersing agent, hard monomer, cationic monomer and molecular weight regulator always add 50%～90% of weight separately, be the add-on of soft monomer in step 3 be soft monomer always add weight 50%～90%, the add-on of hard monomer in step 3 be hard monomer always add weight 50%～90%, the add-on of cationic monomer in step 3 be cationic monomer always add weight 50%～90%, the add-on of molecular weight regulator in step 3 be molecular weight regulator always add weight 50%～90%, the residue amount of initiator that adds then is 50%～80% of total initiator adding weight in the preparation of AKD macromolecule dispersing agent.In actual production, can be according to the needs of producing, get required soft monomer, hard monomer, cationic monomer, molecular weight regulator and initiator in the preparation of this AKD macromolecule dispersing agent respectively ready, and in preparation process 2 and step 3, it is added respectively by additional proportion.
In the preparation, many employing soft monomers, hard monomer, cationic monomer, the preferred weight ratio when molecular weight regulator uses are 30～45: 40～55: 5～15: 0.5～2, can certainly be according to needs of production, carry out suitable adjustment, this is the general knowledge that should know concerning those skilled in the art.
The usage quantity of initiator can adopt relative soft monomer, hard monomer, cationic monomer, 0.5%～2% of molecular weight regulator gross weight, the usage quantity of catalyzer adopts relative soft monomer, hard monomer, cationic monomer, 0.02%～1% of molecular weight regulator gross weight, the usage quantity of acid adopts relative soft monomer, hard monomer, cationic monomer, 2%～20% of molecular weight regulator gross weight, the usage quantity of high molecular polymer adopts relative soft monomer, hard monomer, cationic monomer, 25%～50% of molecular weight regulator gross weight, and can carry out suitable adjustment according to needs of production, this is the general knowledge that should know concerning those skilled in that art; The usage quantity of deionized water can draw according to the concentration of the macromolecule dispersing agent of producing.
Convenient and reliable for whole process of preparation, the preparation of this AKD macromolecule dispersing agent can be adopted and have the speed governing agitator, carry out in the reactor of temperature regulator and condensation reflux device, promptly adopt deionized water, acid, catalyzer and high molecular polymer add and have the speed governing agitator, in the reactor of temperature regulator and condensation reflux device, it is even to be stirred well to system, gradation adds soft monomer then, hard monomer, cationic monomer, molecular weight regulator and initiator carry out prepared in reaction AKD macromolecule dispersing agent, to guarantee effectively intensification in each reactions steps, be incubated and mix.
For better implement the present invention, high molecular polymer comprises as in vinylbenzene maleimide copolymer (SMI), cationic polyvinyl alcohol or the cationic polyacrylamide one or more.
Described acid comprises one or more in Glacial acetic acid, formic acid or the hydrochloric acid.
Described catalyzer comprises one or more in ferrous sulfate, sodium bisulfite, Sodium Pyrosulfite or the S-WAT.
Described soft monomer comprises one or more in butyl acrylate, butyl methacrylate, tert-butyl acrylate, Isooctyl acrylate monomer, Isooctyl methacrylate or the methacrylic tert-butyl acrylate.
Described hard monomer comprises one or more in vinylbenzene, methyl methacrylate, vinyl cyanide or the acrylamide.
Described molecular weight regulator comprises one or more in n-dodecyl mercaptan, uncle's lauryl mercaptan or the mercaptoethanol.
Described cationic monomer comprises one or more in dimethylaminoethyl methacrylate, methylacryoyloxyethyl trimethyl ammonium chloride or the diallyldimethylammonium chloride.
Described initiator comprises one or more in hydrogen peroxide, ammonium persulphate, Potassium Persulphate or the Sodium Persulfate.
Produce a kind of method of cation AKD emulsion and can adopt the cured powder of fusion AKD is joined in the container that fills AKD macromolecule dispersing agent and deionized water and use this AKD macromolecule dispersing agent, be warming up to 75～80 ℃, high speed shear stirs 5～10min and gets emulsion, by a homogeneous, homogenization pressure remains on 24～26MPa then, splashes in the deionized water after cooling afterwards and dilutes, stir simultaneously, after treating that emulsion droplets adds, keep stirring 5～10min, get the cation AKD emulsion.
And in actual production, can adopt the cured powder of molten-bath fusion AKD, in the high speed shear still, contain AKD macromolecule dispersing agent and deionized water and adopt, the cured powder of fusion AKD is joined in the high-shear still that AKD macromolecule dispersing agent and deionized water are housed, heat up, and high-speed stirring gets emulsion, (pressure remains on 24～26MPa) by Homogenizing pump afterwards, entering into the dilution still through supercooler again dilutes, adopt emulsion to drip and start stirring simultaneously, after treating that emulsion droplets adds, keep stirring, discharging afterwards gets the cation AKD emulsion.
The present invention prepares the dispersion agent of positively charged ion styrene-acrylic polymer as AKD with high molecular polymer as protective material, compared with prior art has following advantage and beneficial effect:
(1) dispersion of AKD macromolecule dispersing agent, the emulsifying property excellence of the inventive method production, period of storage is long, and normal temperature is down above 1 year.Use AKD emulsion solid content height (20%～25%) that this dispersion agent produces, electric density height (+35～+ 50mv), grain diameter is little and be evenly distributed.Concentrate between 80nm～600nm median size 156～208nm mostly through NANOPHOX particle-size analyzer particle tested particle diameter.AKD emulsion period of storage is long, and normal temperature is down above 6 months.
(2) product Surface Sizing Properties excellence, down the machine slaking is fast.The double gummed paper result on trial: when AKD emulsion (22.5%) top sizing consumption was 7kg/t paper, following machine was surveyed paper pros and cons Cobb value and is reached 22.5g/m
2And 25g/m
2, picking strength reaches 14 grades (rod wax methods), surveys paper pros and cons Cobb value behind 105 ℃ of oven dry 10min and reaches 21g/m
2And 23g/m
2, surface strength reaches 14 grades (rod wax methods).
(3) synthesis technique is simple, energy consumption is low.Do not add any tensio-active agent in synthesis technique and the product, AKD wax powder only need high-shear disperse about 5min, under 24～26MPa homogeneous once get final product stable prod, no generation of waste materials, environmentally safe.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited in following embodiment.
Embodiment one
The preparation method of this AKD macromolecule dispersing agent,
Materials: 40 weight part SMI (relative molecular mass 20000), 0.05 parts by weight of ferrous sulfate, 15 weight part Glacial acetic acid;
45 parts by weight of styrene, 38 parts by weight of acrylic acid butyl esters, 5 parts by weight of acrylonitrile, 10 weight part dimethylaminoethyl methacrylate, 2 weight part uncle lauryl mercaptans;
Initiator adopts 27.5% hydrogen peroxide by 7.3 weight parts to dissolve in the hydrogen peroxide solution that 23 parts by weight of deionized water are made;
Comprise the following steps and processing condition:
(1) in the reactor that has speed governing agitator, temperature regulator and condensation reflux device, add deionized water, 40 parts of SMI (relative molecular mass 20000), 0.05 part of ferrous sulfate and 15 parts of Glacial acetic acid, fully stir, even to system.
(2) under whipped state in the liquid in step 1, add vinylbenzene, butyl acrylate, vinyl cyanide, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan, the add-on of vinylbenzene, butyl acrylate, vinyl cyanide, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan is and always adds 20% of weight separately, heat temperature raising to 75 ℃, add hydrogen peroxide solution then, add-on is 40% of a hydrogen peroxide solution gross weight, behind the reaction 15min, rises to 78 ℃ again;
(3) in step 2 reaction system, add remaining vinylbenzene, butyl acrylate, vinyl cyanide, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan, vinylbenzene, butyl acrylate, vinyl cyanide, the add-on of dimethylaminoethyl methacrylate and uncle's lauryl mercaptan is and always adds 80% of weight separately, and remaining hydrogen peroxide solution, add-on is 60% of a hydrogen peroxide solution gross weight, vinylbenzene wherein, butyl acrylate, vinyl cyanide, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan joining day are controlled at 2.5h, and the hydrogen peroxide solution dropping time is controlled at 2.75h;
(4) add finish after, again temperature is risen to 85 ℃ of following insulation reaction 2h, be cooled to room temperature, 200 order net filtrations obtain the AKD macromolecule dispersing agent of solid content 25%.
Embodiment two
Materials: 45 weight part SMI (relative molecular mass 10000), 0.06 parts by weight of ferrous sulfate, 17 weight part Glacial acetic acid;
40 parts by weight of styrene, 40 weight part butyl methacrylate, 5 parts by weight of methylmethacrylate, 13 weight part dimethylaminoethyl methacrylate, 2 weight part uncle lauryl mercaptans;
Initiator adopts 27.5% hydrogen peroxide by 7.7 weight parts to dissolve in the hydrogen peroxide solution that 23 parts by weight of deionized water are made;
Comprise the following steps and processing condition:
(1) add deionized water, 45 parts of SMI, 0.06 part of ferrous sulfate and 17 parts of Glacial acetic acid in the reactor that has speed governing agitator, temperature regulator and condensation reflux device, it is even to be stirred well to system;
(2) under whipped state in the liquid in step 1, add vinylbenzene, butyl methacrylate, methyl methacrylate, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan, the add-on of vinylbenzene, butyl methacrylate, methyl methacrylate, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan is and always adds 20% of weight separately, heating systems, be warming up to 75 ℃, add hydrogen peroxide solution then, add-on is 40% of a hydrogen peroxide solution gross weight, behind the stirring reaction 15min, rise to 78 ℃ again;
(3) in step 2 reaction system, add remaining vinylbenzene, butyl methacrylate, methyl methacrylate, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan, vinylbenzene, butyl methacrylate, methyl methacrylate, the add-on of dimethylaminoethyl methacrylate and uncle's lauryl mercaptan is and always adds 80% of weight separately, and residue hydrogen peroxide solution, add-on is 60% of a hydrogen peroxide solution gross weight, vinylbenzene wherein, butyl methacrylate, methyl methacrylate, dimethylaminoethyl methacrylate and uncle's lauryl mercaptan joining day are controlled at 2.5h, the hydrogen peroxide solution dropping time is controlled at 2.75h
(4) after adding finishes, again temperature is risen to 85 ℃ of following insulation reaction 2h, be cooled to room temperature, filter, obtain the AKD macromolecule dispersing agent of solid content 25%.
Embodiment three
Materials: 40 weight part SMI (relative molecular mass 20000), 0.05 parts by weight of ferrous sulfate, 15 weight part Glacial acetic acid;
45 parts by weight of styrene, 40 parts by weight of acrylic acid butyl esters, 6 parts by weight of acrylonitrile, 1 weight part uncle lauryl mercaptan;
Cationic monomer adopts 8 weight part methylacryoyloxyethyl trimethyl ammonium chlorides to dissolve in the cation mono liquid solution of making in 10 parts by weight of deionized water;
Initiator adopts 27.5% hydrogen peroxide by 7.5 weight parts to dissolve in the hydrogen peroxide solution that 23 parts by weight of deionized water are made;
Comprise the following steps and processing condition:
(1) add deionized water, 40 weight part SMI, 0.05 parts by weight of ferrous sulfate and 15 weight part Glacial acetic acid in the reactor that has speed governing agitator, temperature regulator and condensation reflux device, it is even to be stirred well to system;
(2) under whipped state in the liquid in step 1, add vinylbenzene, butyl acrylate, vinyl cyanide, uncle's lauryl mercaptan and cation mono liquid solution, wherein the add-on of vinylbenzene, butyl acrylate, vinyl cyanide, uncle's lauryl mercaptan is and always adds 20% of weight separately, cation mono liquid solution add-on is 20% of a gross weight, heat temperature raising to 75 ℃, add hydrogen peroxide solution then, add-on be hydrogen peroxide solution always add weight 40%, behind the stirring reaction 15min, rise to 78 ℃ again;
(3) in step 2 reaction system, add remaining vinylbenzene, butyl acrylate, vinyl cyanide, uncle's lauryl mercaptan and cation mono liquid solution respectively, and remaining hydrogen peroxide solution, vinylbenzene, butyl acrylate, vinyl cyanide and uncle's lauryl mercaptan add-on be and always add 80% of weight separately, cation mono liquid solution add-on is 80% of a cationic monomer total solution weight, and the hydrogen peroxide solution add-on is 60% of a hydrogen peroxide solution gross weight; Wherein vinylbenzene, butyl acrylate, vinyl cyanide, uncle's lauryl mercaptan and cation mono liquid solution joining day are controlled at 2.5h, and the hydrogen peroxide solution dropping time is controlled at 2.75h;
(4) add finish after, again temperature is risen to 85 ℃ of following insulation reaction 2.5h, be cooled to room temperature, 200 order net filtrations obtain the AKD macromolecule dispersing agent of solid content 25%.
Embodiment four
Materials: 45 weight part cationic polyvinyl alcohols (relative molecular mass 8800), 0.3 weight part S-WAT, 8 weight part formic acid;
40 parts by weight of acrylonitrile, the 40 parts by weight of acrylic acid tert-butyl esters, 5 parts by weight of methylmethacrylate, 13 weight part diallyldimethylammonium chlorides, 2 weight part mercaptoethanols;
Cationic monomer adopts 13 weight part methylacryoyloxyethyl trimethyl ammonium chlorides to dissolve in the cation mono liquid solution of making in 10 parts by weight of deionized water;
Initiator adopts the ammonium persulphate by 0.6 weight part to dissolve in the ammonium persulfate solution that 23 parts by weight of deionized water are made;
Comprise the following steps and processing condition:
(1) add deionized water, 45 weight part cationic polyvinyl alcohols, 0.35 weight part S-WAT, 8 weight part formic acid in the reactor that has speed governing agitator, temperature regulator and condensation reflux device, it is even to be stirred well to system;
(2) under whipped state in the liquid in step 1, add vinyl cyanide, tert-butyl acrylate, methyl methacrylate, mercaptoethanol and cation mono liquid solution, the add-on of vinyl cyanide, tert-butyl acrylate, methyl methacrylate, mercaptoethanol is and always adds 10% of weight separately, cation mono liquid solution add-on is 10% of a cationic monomer total solution weight, heating systems, be warming up to 73 ℃, add ammonium persulfate solution then, add-on is 50% of an ammonium persulfate solution gross weight, behind the stirring reaction 17min, rise to 78 ℃ again;
(3) in step 2 reaction system, add remaining vinyl cyanide, tert-butyl acrylate, methyl methacrylate, mercaptoethanol and cation mono liquid solution, vinyl cyanide, tert-butyl acrylate, methyl methacrylate, the add-on of mercaptoethanol is and always adds 90% of weight separately, cation mono liquid solution add-on is 90% of a cationic monomer total solution weight, and residue ammonium persulfate solution, add-on is 50% of an ammonium persulfate solution gross weight, vinyl cyanide wherein, tert-butyl acrylate, methyl methacrylate, mercaptoethanol and cation mono liquid solution joining day are controlled at 2h, the ammonium persulfate solution dropping time is controlled at 2.5h
(4) after adding finishes, again temperature is risen to 80 ℃ of following insulation reaction 3h, be cooled to room temperature, filter, obtain the AKD macromolecule dispersing agent of solid content 25%.
Embodiment five
Materials: 45 weight part cationic polyacrylamides (relative molecular mass 6200), 0.6 weight part sodium bisulfite, 5 weight part hydrochloric acid;
40 parts by weight of styrene, the different monooctyl ester of 40 parts by weight of acrylic acid, 5 parts by weight of methylmethacrylate, 13 weight part dimethylaminoethyl methacrylate, 2 weight part n-dodecyl mercaptans;
Initiator adopts the Potassium Persulphate by 0.6 weight part to dissolve in the potassium persulfate solution that 23 parts by weight of deionized water are made;
Comprise the following steps and processing condition:
(1) add deionized water, 45 weight part cationic polyacrylamides, 0.7 weight part sodium bisulfite, 5 weight part hydrochloric acid in the reactor that has speed governing agitator, temperature regulator and condensation reflux device, it is even to be stirred well to system;
(2) under whipped state in the liquid in step 1, add vinylbenzene, Isooctyl acrylate monomer, methyl methacrylate, dimethylaminoethyl methacrylate and n-dodecyl mercaptan, the add-on of vinylbenzene, Isooctyl acrylate monomer, methyl methacrylate, dimethylaminoethyl methacrylate and n-dodecyl mercaptan is and always adds 30% of weight separately, heating systems, be warming up to 74 ℃, add potassium persulfate solution then, add-on is 40% of a potassium persulfate solution gross weight, behind the stirring reaction 13min, rise to 77 ℃ again;
(3) in step 2 reaction system, add remaining vinylbenzene, Isooctyl acrylate monomer, methyl methacrylate, dimethylaminoethyl methacrylate and n-dodecyl mercaptan, vinylbenzene, Isooctyl acrylate monomer, methyl methacrylate, the add-on of dimethylaminoethyl methacrylate and n-dodecyl mercaptan is and always adds 70% of weight separately, and residue potassium persulfate solution, add-on is 60% of a potassium persulfate solution gross weight, vinylbenzene wherein, Isooctyl acrylate monomer, methyl methacrylate, dimethylaminoethyl methacrylate and n-dodecyl mercaptan joining day are controlled at 2.75h, and the potassium persulfate solution dropping time is controlled at 3h;
(4) after adding finishes, again temperature is risen to 82 ℃ of following insulation reaction 2.5h, be cooled to room temperature, filter, obtain the AKD macromolecule dispersing agent of solid content 25%.
Embodiment six
Adopt the AKD macromolecule dispersing agent of embodiment one preparation to prepare the AKD emulsion, comprise the following steps and processing condition:
The cured powder of 160 weight part AKD is joined in the molten-bath, 60～65 ℃ of following fusions; 128 weight part AKD emulsifying agents and 185 parts by weight of deionized water are added in the high-shear still, be warming up to and add the good cured powder of AKD of fusion after 70 ℃, stop heating after rising to 78 ℃ again, (2900 commentaries on classics/min) disperse 5min then by a Homogenizing pump (pressure remains on 26MPa), join in the dilution still that adds 460 parts by weight of deionized water through supercooler in the high speed shear stirring, start stirring simultaneously, after treating that emulsion droplets adds, keep stirring 10min, discharging gets the 20%AKD emulsion.
Embodiment seven
Adopt the AKD macromolecule dispersing agent of embodiment two preparations to prepare the AKD emulsion, comprise the following steps and processing condition:
The cured powder of 160 weight part AKD is joined in the molten-bath, 60～65 ℃ of following fusions; 128 weight part AKD macromolecule dispersing agents and 185 parts by weight of deionized water are added in the high-shear still, be warming up to and add the good cured powder of AKD of fusion after 70 ℃, stop heating after rising to 80 ℃ again, (2900 change/min) disperse 10min to open the high speed shear stirring, then by a Homogenizing pump (pressure remains on 24MPa), join in the dilution still that adds 370 parts by weight of deionized water through supercooler, start stirring simultaneously, after treating that emulsion droplets adds, keep stirring 5min, discharging gets the 22.5%AKD emulsion.
Embodiment eight
Adopt the AKD macromolecule dispersing agent of embodiment three preparations to prepare the AKD emulsion, comprise the following steps and processing condition:
Comprise the following steps and processing condition:
The cured powder of 160 weight part AKD is joined in the molten-bath, 60～65 ℃ of following fusions; 128 weight part AKD macromolecule dispersing agents and 185 parts by weight of deionized water are added in the high-shear still, be warming up to and add the good cured powder of AKD of fusion after 70 ℃, stop heating after rising to 76 ℃ again, (2900 commentaries on classics/min) disperse 8min then by an equal Homogenizing pump (pressure remains on 25MPa), enter in the dilution still that adds 460 parts by weight of deionized water through supercooler to open high-speed stirring, start stirring simultaneously, after treating that emulsion droplets adds, keep stirring 8min, discharging gets the 20%AKD emulsion.
Embodiment nine
The application of this cation AKD emulsion surface sizing agent:
Product of the present invention (22.5%AKD emulsion) is tried out on 1760mm double gummed paper machine, and is now contrasted application result such as table 1 with the glue-applying technique effect with paper plant.
Paper plant has technology now: AKD (13.5%) neutral sizing agent consumption 12kg/t paper, Surface Size (25%) consumption 4.5kg/t paper in the slurry, adopt Sumstar 190 and the applying glue of Surface Size (25%) blending surface, surface size concentration 6%, 65 ℃ of applying glue temperature, ton paper gluing agents cost amounts to 65 yuan.Use product technology of the present invention: 22.5%AKD product consumption 7kg/t paper, no internal sizing agent adopts Sumstar 190 and the applying glue of 22.5%AKD product blending surface, surface size concentration 6%, 65 ℃ of applying glue temperature, ton paper gluing agents cost amounts to 63 yuan.
The application result of table 1 product on double gummed paper
| The double gummed paper performance index | Existing technology | Use product technology of the present invention |
| Quantitative (g/m 2) | 60 | 61 |
| Just/reverse side Cobb value (g/m 2) | 24.5/28 | 22.5/25 |
| Picking strength (rod wax method) | 14 | 14 |
| Just/reverse side smoothness (s) | 48/42 | 52/49 |
| Fracture length (km) | 3.9 | 4.0 |
| Burst index (kPa.m 2/g) | 2.9 | 3.1 |
As shown in Table 1, under the close situation of ton paper gluing agents cost, use product of the present invention (22.5%AKD emulsion) effect to be better than existing technology.
As mentioned above, just can realize the present invention preferably.
Claims (10)
1, a kind of preparation method of AKD macromolecule dispersing agent is characterized in that comprising step:
1) acid, catalyzer and high molecular polymer are mixed with deionized water, it is even to be stirred well to system;
2) under the whipped state in the liquid in step 1, add part soft monomer, hard monomer, cationic monomer and molecular weight regulator, heat temperature raising to 73～75 ℃ add the part initiator then, behind insulation 13～17min, are warming up to 76～80 ℃;
3) in step 2 reaction system, drip soft monomer, hard monomer, cationic monomer, molecular weight regulator and the remainder initiator of remainder, wherein soft monomer, hard monomer, cationic monomer and molecular weight regulator dropping time are controlled at 2～3h, and the initiator dropping time is controlled at 2.5～3h;
4) dropwise, again temperature is risen to 80～85 ℃ of following insulation reaction 2～3h, be cooled to room temperature, filter and promptly obtain product;
Wherein, the add-on of soft monomer, hard monomer, cationic monomer and molecular weight regulator is respectively soft monomer, hard monomer, cationic monomer and molecular weight regulator and always adds 10%～50% of weight separately in the step 2, the add-on of initiator be initiator always add weight 20%～50%; The amount that adds remaining soft monomer, hard monomer, cationic monomer and molecular weight regulator in the step 3 is respectively soft monomer, hard monomer, cationic monomer and molecular weight regulator and always adds 50%～90% of weight separately, adds the residue amount of initiator and be that initiator always adds weight 50%～80%.
2, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described high molecular polymer comprises one or more in SMI, cationic polyvinyl alcohol or the cationic polyacrylamide.
3, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described acid comprises one or more in Glacial acetic acid, formic acid or the hydrochloric acid.
4, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described catalyzer comprises one or more in ferrous sulfate, sodium bisulfite, Sodium Pyrosulfite or the S-WAT.
5, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described soft monomer comprises one or more in butyl acrylate, butyl methacrylate, tert-butyl acrylate, Isooctyl acrylate monomer, Isooctyl methacrylate or the methacrylic tert-butyl acrylate.
6, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described hard monomer comprises one or more in vinylbenzene, methyl methacrylate, vinyl cyanide or the acrylamide.
7, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described molecular weight regulator comprises one or more in n-dodecyl mercaptan, uncle's lauryl mercaptan or the mercaptoethanol.
8, by the preparation method of the described AKD macromolecule dispersing agent of claim 1, it is characterized in that: described cationic monomer comprises one or more in dimethylaminoethyl methacrylate, methylacryoyloxyethyl trimethyl ammonium chloride or the diallyldimethylammonium chloride.
9, by the preparation method of each described AKD macromolecule dispersing agent in the claim 1 to 8, it is characterized in that: described initiator comprises one or more in hydrogen peroxide, ammonium persulphate, Potassium Persulphate or the Sodium Persulfate.
10, the AKD macromolecule dispersing agent of the described AKD macromolecule dispersing agent of claim 1 preparation method preparation is used for synthesizing cationic AKD emulsion, it is characterized in that: the cured powder of fusion AKD is joined in the container that fills AKD macromolecule dispersing agent and deionized water, be warming up to 75～80 ℃, high speed shear stirs 5～10min and gets emulsion, then by a homogeneous, homogenization pressure remains on 24～26MPa, after cooling, splash in the deionized water afterwards and dilute, stir simultaneously, after treating that emulsion droplets adds, keep stirring 5～10min, get the cation AKD emulsion.
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