CN109293827B - Process for the preparation of bead-like cationic polyacrylamide retention aids and their use for retention of pulp slurries - Google Patents
Process for the preparation of bead-like cationic polyacrylamide retention aids and their use for retention of pulp slurries Download PDFInfo
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- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/41—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups
- D21H17/44—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing ionic groups cationic
- D21H17/45—Nitrogen-containing groups
- D21H17/455—Nitrogen-containing groups comprising tertiary amine or being at least partially quaternised
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/06—Paper forming aids
- D21H21/10—Retention agents or drainage improvers
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Abstract
The invention relates to a preparation method of bead-shaped cationic polyacrylamide retention aid and retention application of the bead-shaped cationic polyacrylamide retention aid to paper pulp slurry, wherein a reverse emulsion polymerization method is utilized, and a reaction micro-environment cavity in an acrylamide polymerization process is accurately regulated and controlled, so that the molecular weight and the polymerization mode of acrylamide are effectively regulated and controlled, the physical form of a PAM product is controlled, and a microbead-shaped PAM product which is easy to disperse and has the diameter of 0.8-1.5 mm is obtained. The micro-bead PAM avoids the phenomenon of water agglomeration, can greatly increase the dissolution speed of the PAM in water, and solves the dust pollution caused by powder PAM, thereby simplifying the adding process, reducing the requirement on equipment, reducing the production cost and being beneficial to the application of large-scale commercialization.
Description
Technical Field
The invention relates to a preparation method of bead-shaped cationic polyacrylamide retention aid and retention application of the retention aid to paper pulp slurry, belonging to the field of preparation of water-soluble high molecular compounds.
Background
In the field of papermaking, the retention aid improves the retention rate of fine fibers, fillers and the like by changing the flocculation state of papermaking pulp, thereby achieving the results of reducing the loss of the fibers and the fillers and reducing pollution load. With the high speed of paper making technology and the higher requirements on product quality, new efficient retention systems and retention technologies corresponding to the technology must be used to ensure the rapid development of the paper making industry. Among them, Polyacrylamide (PAM) and its graft copolymer products of different ion types are one of representative papermaking retention aids at present.
PAM is a water-soluble organic high molecular compound, and the main chain contains active amide groups and double bonds. Different polymerization processes are adopted, different functional groups are introduced, and PAM series products with different molecular weights and different charge densities can be obtained. PAM has the characteristics of large molecular weight, enough reactive active points on molecular chains and the like, can be combined with fibers, fillers and the like, and has a combination mechanism of mainly neutralizing opposite charges; part of chain segments are adsorbed on the surfaces of the particles in a mosaic shape to be crosslinked or bridged; the polymer chains form an entangled network, trapping the particles, forming various cross-linked networks, and achieving the retention effect. And meanwhile, PAM can improve the drainage performance of the net paper stock and the retention rate of the fine fibers and the filler. The fines (including fines and fillers) in the stock adhere to the surface of the longer fibers and form flocks of greater volume, making the stock easier to dewater and reducing the loss of fines through the wire.
Various PAM products used for the papermaking retention aid at present are mostly in powder shape, the phenomenon of deliquescence and caking is easy to occur in the storage process, and meanwhile, the powder PAM is easy to generate dust pollution in the use process and is not beneficial to environmental protection; in the papermaking process, the powdered PAM is easy to agglomerate when meeting water in the adding process, the dissolving time is long, the dissolving time is generally more than 1 hour, the use efficiency of the PAM in water is greatly limited, and the efficiency improvement of the papermaking process is not facilitated. Therefore, it is necessary to develop a method for producing instant PAM.
In order to solve the problems of low PAM dissolving efficiency and dust pollution, one method is to control the polymerization microenvironment of the macromolecule by regulating the synthesis process of the macromolecule polymer to obtain the macromolecule microbeads with controllable shapes, so as to reduce the agglomeration phenomenon of molecules in the solvent. Chinese patent CN102327761A reports a method for obtaining a composite polymer microbead by using a microfluid reactor to control the environment of high molecular polymerization. The polymer microsphere has good dispersibility, and can be widely applied to the fields of drug carrier release and the like.
According to the invention, by using a reverse emulsion polymerization method, the molecular weight and the polymerization mode of acrylamide are effectively regulated and controlled by accurately regulating and controlling a reaction micro-environment cavity in the polymerization process of the acrylamide, so that the physical form of the PAM product is controlled, and the microbead-shaped PAM product which is easy to disperse and has the diameter of 0.8-1.5 mm is obtained. The micro-bead PAM avoids the phenomenon of water agglomeration, can greatly increase the dissolution speed of the PAM in water, and solves the dust pollution caused by powder PAM, thereby simplifying the adding process, reducing the requirement on equipment, reducing the production cost and being beneficial to the application of large-scale commercialization.
Disclosure of Invention
Aiming at the defects of the PAM at present, the invention provides a method for utilizing an inverse emulsion polymerization method; the multi-step initiation polymerization is carried out at different temperatures by utilizing a plurality of initiators to obtain the bead cationic polyacrylamide with controllable diameter, 0.8-1.5 mm of particle diameter, about 1-2mm of average size, smooth particle appearance and very high solubility and dissolution speed in water. Compared with the similar PAM retention aid under the condition of the same dosage, the bead cationic PAM has excellent pulp drainage performance and retention effect of papermaking chemicals; and the preparation method has the advantages of safety, simplicity, low cost, environmental friendliness and the like.
The technical scheme of the invention is as follows:
a method for preparing bead cationic polyacrylamide retention aid, which is characterized by comprising the following steps:
preparation of an aqueous phase: dissolving acrylamide solid with water, adding cationic ethylene polymer monomer, and forming transparent monomer water solution at 40-45 deg.C;
selecting ammonium persulfate (initiator A), V50 (chemical name of V50 is 2, 2' -azobisisobutyl ether dihydrochloride, initiator B) and VA044 (chemical name of VA044 is azodiisopropyl imidazoline hydrochloride and initiator C), preparing one, two or three water-soluble composite initiators into a water-phase initiator (hereinafter initiator D), and adding all the water-soluble composite initiators into the monomer aqueous solution at one time to mix uniformly to prepare a water phase;
preparing an oil phase: adding surfactant Span-60 and Span-80(Span-60 is sorbitan monostearate; Span-80 is sorbitan fatty acid ester) and initiator V-60 (chemical name of V-60 is azodiisobutyronitrile), and cyclohexane or methylcyclohexane or mixed solvent of the two, the volume of which is 1-3 times of that of the above-mentioned water phase, into a reaction container equipped with stirrer, condenser and nitrogen gas conduit to prepare transparent oil phase;
polymerization reaction: and (3) respectively carrying out nitrogen deoxidization on the two systems (water phase and oil phase), raising the temperature of the oil phase to 40-45 ℃ under the protection of nitrogen, and then dripping the water phase into the oil phase at the speed of 1-10 ml per minute by using a syringe pump. After the water phase is added, preserving heat for 0.5-1h at 40-45 ℃, then quickly heating to 60-70 ℃, preserving heat for 2-4 h at the temperature, finally heating to 75-80 ℃, continuing to react for 0.5-1h, and finishing the reaction;
and (3) post-treatment: and after the reaction is finished, filtering the product by using a Buchner funnel, and drying the product in a hot air oven at the temperature of 60-65 ℃ to obtain the bead-shaped cationic polyacrylamide retention aid.
The synthesis route of the bead cationic PAM product is illustrated by taking Poly (AM-DMC) as an example:
in a preferred embodiment, the total solubility of the acrylamide AM and the cationic vinyl polymer monomer in the transparent aqueous monomer solution is preferably 1-5 g/ml.
In a preferred embodiment, the cationic vinylic polymeric monomer described herein is selected from the group consisting of dimethyldiallylammonium chloride (DMDAAC), methacryloyloxyethyltrimethylammonium chloride (DMC), acryloyloxyethyltrimethylammonium chloride (DAC).
In a preferred embodiment, the weight ratio of acrylamide monomer to cationic vinyl polymer monomer is preferably from 25% to 75% to 25%.
In another preferred embodiment of the present invention, the weight ratio of the acrylamide monomer to the cationic vinyl-based polymer monomer is more preferably 35% to 65% to 35%.
In a preferred embodiment, the organic solvent is 1 to 3 times the volume of the aqueous dispersant.
In the preparation method, the stirring speed of the polymerization reaction is 100-600 r/min.
In another preferred embodiment of the present invention, the weight ratio of Span-60/Span-80 is 1: 4 to 4: 1.
In another preferred embodiment of the present invention, the amount of the initiator D used in the preparation of the aqueous phase is 0.5 to 2 wt% based on the total weight of the monomers (acrylamide and cationic vinyl polymer monomer).
In another preferred embodiment of the present invention, the amount of the surfactants Span-60 and Span-80 is 5 to 100% by weight of the oil phase.
In another preferred embodiment of the invention, the ratio by weight of the initiator V-60 to the initiator D is from 50% to 200%.
In another preferred embodiment of the present invention, the solution remaining after obtaining the bead-like cationic polyacrylamide is subjected to liquid separation to obtain an aqueous phase and an oil phase, wherein the aqueous phase and the oil phase can be recycled.
The particle size and shape of polyacrylamide were observed and measured by a polarizing microscope, and the solid content of polyacrylamide was measured by the measurement method of GBT 12005.2-1989.
The method adopts water-in-oil reversed-phase suspension polymerization, adopts multistep temperature rise to control the polymerization speed, and important control steps comprise placing different types of initiators in different reaction phases to ensure the maximum dispersion of the initiators; the initial temperature of the system is set at 40-45 ℃, the dosage and the temperature of the initiator are controlled, and the polymerization volume of the water-in-oil reversed phase suspension polymerization is well controlled, so that the coordination effect of the composite initiator is greatly improved. The beaded polyacrylamide obtained by the preparation method has very good dissolution efficiency in water, and compared with similar PAM retention aids, the beaded PAM has better pulp drainage performance and retention performance of papermaking chemicals.
The present application is obviously different from the prior art inventions, and mainly comprises:
the method adopts reversed phase suspension polymerization, simultaneously controls the dosage and the system of an initiator, utilizes an injection pump to add a water phase into an oil phase, ensures that the oil phase is not locally supersaturated, ensures that the polymerization can be controllably and stably carried out at a certain temperature, and simultaneously utilizes the characteristic of water-in-oil to obtain a micro-polymerization unit with controllable volume by utilizing stirring speed and a dispersing agent to obtain bead cationic PAM. DAC and AM with good performance are selected for copolymerization, and the retention aid with good performance is obtained.
Detailed Description
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
EXAMPLE 1 preparation of bead cationic Polyacrylamide Retention aid
Preparation of an aqueous phase: weighing 14.5g of Acrylamide (AM) and 4.5g of cationic monomer acryloyloxyethyl trimethyl ammonium chloride (DAC), dissolving in 50ml of deionized water at 40-45 ℃ to form a transparent monomer aqueous solution, then adding 0.015g of initiator V-50 and ammonium persulfate (the weight ratio is 1: 1), and uniformly mixing to prepare a water phase;
preparing an oil phase: weighing 0.80g of emulsifier Span-60, 0.80g of emulsifier Span-80 and 0.20g of initiator V60 azobisisobutyronitrile, putting the mixture into a 500mL four-neck round bottom flask provided with a mechanical stirrer, a condenser tube and a nitrogen conduit, adding 200mL of cyclohexane, introducing condensed water, stirring, heating to 45 ℃ until the emulsifier and the initiator are completely dissolved to form a transparent oil phase;
polymerization reaction: respectively carrying out nitrogen deoxidization on two systems (water phase and oil phase), uniformly stirring in a constant-temperature water bath at 45 ℃ in a four-neck round-bottom flask (the stirring speed is 150r/min), introducing nitrogen to remove oxygen for 30min, slowly injecting the water phase into the oil phase at the speed of 2ml/min by using an injection pump, introducing condensed water, keeping the reaction temperature at 45 ℃ at the beginning, quickly heating to 65 ℃ after stirring for 0.5-1h, reacting for 3h at the temperature, heating to 75 ℃ to continue reacting for 0.5h until the reaction is finished, and keeping the stirring speed constant in the whole reaction process, wherein the stirring speed is 150 r/min;
and (3) post-treatment: after the reaction, the stirring was stopped, the granular polymer settled to the bottom of the flask, the product was filtered dry using a buchner funnel and dried in a hot air oven at 60 ℃ to obtain a retention aid Poly (AM-DAC) in the form of beads with a diameter of 1.3 ± 0.2mm and a solid content of 93%.
EXAMPLE 2 preparation of bead Polyacrylamide Retention aid
The same procedures as in example 1 were repeated except that the amount of the initiator used in the aqueous phase preparation step was changed to V-50 and 0.03g (weight ratio: 1) based on ammonium persulfate to give a retention aid Poly (AM-DAC) in the form of beads having a diameter of 1.0. + -. 0.2mm and a solid content of 90%.
EXAMPLE 3 preparation of bead Polyacrylamide Retention aid
The same procedures as in example 1 were repeated except that the initiator in the aqueous phase preparation step was changed to VA044 in an amount of 0.03g (weight ratio: 1) based on ammonium persulfate and, as an alternative, a retention aid Poly (AM-DAC) in the form of beads having a diameter of 1.1. + -. 0.2mm and a solids content of 91% was obtained.
EXAMPLE 4 preparation of bead Polyacrylamide Retention aid
The same conditions as in example 1 were repeated except that the initiator used in the preparation of the aqueous phase was changed to 0.03g (1: 1 weight ratio) based on VA044 and V50, to give a retention aid Poly (AM-DAC) in the form of beads having a diameter of 1.3. + -. 0.2mm and a solids content of 88%.
EXAMPLE 4 preparation of bead Polyacrylamide Retention aid
The same procedures as in example 1 were repeated except that the cationic monomer in the aqueous phase preparation step was changed from 4.5g of the cationic monomer acryloyloxyethyltrimethylammonium chloride (DAC) in example 1 to 4.8g of methacryloyloxyethyltrimethylammonium chloride (DMC), to obtain a retention aid Poly (AM-DMC) in the form of beads having a diameter of 1.1. + -. 0.2mm and a solid content of 88%.
EXAMPLE 5 preparation of bead-like Polyacrylamide Retention aid
The same procedures as in example 4 were repeated except that the initiator in the aqueous phase preparation step was changed to V-50 and 0.03g (weight ratio: 1) based on ammonium persulfate to obtain a retention aid Poly (AM-DMC) in the form of beads having a diameter of 1.1. + -. 0.2mm and a solid content of 85%.
EXAMPLE 6 preparation of bead Polyacrylamide Retention aid
The same conditions as in example 4 were followed except that the initiator in the aqueous phase preparation step was changed to 0.03g (weight ratio: 1) based on VA044 and ammonium persulfate to give a retention aid Poly (AM-DMC) in the form of beads having a diameter of 1.1. + -. 0.2mm and a solids content of 83%.
EXAMPLE 7 preparation of bead-like Polyacrylamide Retention aid
The same conditions as in example 4 were followed except that the amount of the initiator used in the aqueous phase preparation step was changed to 0.03g (1: 1 weight ratio) based on VA044 and V50, to give a retention aid Poly (AM-DMC) in the form of beads having a diameter of 1.3. + -. 0.2mm and a solids content of 82%.
EXAMPLE 8 preparation of bead Polyacrylamide Retention aid
The same procedures as in example 1 were repeated except that the cationic monomer in the aqueous phase preparation step was changed from 4.5g of the cationic monomer acryloyloxyethyltrimethylammonium chloride (DAC) in example 1 to 4.9g of dimethyldiallylammonium chloride (DMDAAC), to obtain a retention aid Poly (AM-DMDAAC) in the form of beads having a diameter of 1.2. + -. 0.2mm and a solid content of 86%.
EXAMPLE 9 preparation of bead Polyacrylamide Retention aid
The same procedures as in example 8 were repeated except that the initiator in the aqueous phase preparation step was changed to VA044 in an amount of 0.03g (weight ratio: 1) based on ammonium persulfate and, as an alternative, Poly (AM-DMDAAC) as a retention aid in the form of beads having a diameter of 1.2. + -. 0.2mm and a solid content of 83%.
EXAMPLE 10 preparation of bead-like Polyacrylamide Retention aid
The same conditions as in example 8 were followed except that the initiator used in the aqueous phase preparation step was changed to 0.03g (weight ratio: 1) based on VA044 and V50, to give a retention aid Poly (AM-DMDAAC) in the form of beads having a diameter of 1.1. + -. 0.2mm and a solids content of 80%.
EXAMPLE 11 preparation of bead Polyacrylamide Retention aid
The same conditions as in example 1 were repeated except that the organic solvent in the oil phase preparation step was changed to methylcyclohexane, to obtain a retention aid Poly (AM-DMDAAC) in the form of beads having a diameter of 1.2. + -. 0.2mm and a solid content of 83%.
EXAMPLE 12 Performance testing of bead Polyacrylamide Retention aid
First, sample preparation
1. Experiment slurry: pulp slurry without added chemicals.
2. Experimental drugs: the bead-shaped polyacrylamide retention aid is prepared by the following steps of firstly, preparing the bead-shaped polyacrylamide retention aid, and secondly, preparing other products in the same industry.
3. Dissolution concentration of experimental drug: 0.1 percent.
4. An experimental instrument: BTG DFR-05 dynamic water filter
Second, sample test
Under the condition of selecting the same dosage, the dosage of the retention aid is as follows: 200g/t, simulating the production conditions of a paper machine in a laboratory through a DFR-05 dynamic drainage instrument, testing the drainage performance of paper pulp and evaluating the retention effect of papermaking chemicals. The retention rate can be automatically displayed during testing.
Third, test results
| Test 1 | Test 2 | Test 3 | Comparative experiment 1 | Comparative experiment 2 | |
| Retention rate% | 62.3 | 62.9 | 62.8 | 61.3 | 61.6 |
| Water filtration g | 599 | 602 | 594 | 546 | 548 |
Note: runs 1-3 used the bead polyacrylamide retention aid described in examples 1-3 of the present application, respectively, run 1 used the french elsen 4910 and run 2 used the polyacrylamide commercially available from basf Percol47, germany.
The data in the table above show that with the bead polyacrylamide retention aid described herein, the retention and drainage of the slurry are increased to varying degrees, with a significant increase in drainage.
Claims (6)
1. A method for preparing bead cationic polyacrylamide retention aid, which is characterized by comprising the following steps:
preparation of an aqueous phase: dissolving acrylamide solid with water, adding cationic ethylene polymer monomer, and forming transparent monomer water solution at 40-45 deg.C; selecting one, two or three of ammonium persulfate, 2' -azobisisobutyl ether dihydrochloride and azodiisopropyl imidazoline hydrochloride to prepare a water phase initiator D, and adding all the initiators into the monomer aqueous solution at one time to mix uniformly to prepare a water phase; the cationic vinyl polymer monomer is selected from dimethyl diallyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride or acryloyloxyethyl trimethyl ammonium chloride;
preparing an oil phase: adding surfactants Span-60 and Span-80 and an initiator V-60 and methylcyclohexane or a mixed solvent of cyclohexane and methylcyclohexane, the volume of which is 1-3 times of the volume of the water phase, into a reaction vessel provided with a stirrer, a condenser tube and a nitrogen conduit to prepare a transparent oil phase;
polymerization reaction: respectively carrying out nitrogen deoxidization on the water phase and the oil phase of the two systems, raising the temperature of the oil phase to 40-45 ℃ under the protection of nitrogen, and then dripping the water phase into the oil phase at the speed of 1-10 ml per minute by using an injection pump; after the water phase is added, preserving heat for 0.5-1h at 40-45 ℃, then quickly heating to 60-70 ℃, preserving heat for 2-4 h at the temperature, finally heating to 75-80 ℃, continuing to react for 0.5-1h, and finishing the reaction;
and (3) post-treatment: after the reaction is finished, filtering the product by using a Buchner funnel, and drying the product in a hot air oven at 60-65 ℃ to obtain the bead-shaped cationic polyacrylamide retention aid with the particle diameter size of 0.8-1.5 mm.
2. The production method according to claim 1, characterized in that: the weight ratio of the acrylamide monomer to the cationic vinyl polymer monomer is (35 percent: 65 percent) to (65 percent: 35 percent).
3. The production method according to claim 1, characterized in that: the weight ratio of Span-60 to Span-80 is (1: 4) - (4: 1).
4. The production method according to claim 1, characterized in that: in the water phase preparation process, the dosage of the initiator D is 0.5-2 wt% of the total weight of the acrylamide and the cationic ethylene polymer monomer.
5. The production method according to claim 1, characterized in that: the amount of the surfactant Span-60 and Span-80 is more than 5 percent of the weight of the oil phase.
6. The production method according to claim 1, characterized in that: and (3) separating the solution remained after the pearl cationic polyacrylamide is obtained to obtain a water phase and an oil phase, wherein the water phase and the oil phase are recycled.
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| JP2007154349A (en) * | 2005-12-02 | 2007-06-21 | Harima Chem Inc | Method for producing paperboard |
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| WO2001051707A1 (en) * | 2000-01-12 | 2001-07-19 | Calgon Corporation | The use of inorganic sols in the papermaking process |
| JP2007154349A (en) * | 2005-12-02 | 2007-06-21 | Harima Chem Inc | Method for producing paperboard |
| CN101628953A (en) * | 2009-08-11 | 2010-01-20 | 华南师范大学 | High molecular weight cationic polyacrylamide preparation method |
| CN107208376A (en) * | 2015-01-27 | 2017-09-26 | 凯米罗总公司 | Polymeric articles of particle form and application thereof |
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