CN101962425B - Dendrimer-star anionic trash catcher and application thereof - Google Patents
Dendrimer-star anionic trash catcher and application thereof Download PDFInfo
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- CN101962425B CN101962425B CN2010102779036A CN201010277903A CN101962425B CN 101962425 B CN101962425 B CN 101962425B CN 2010102779036 A CN2010102779036 A CN 2010102779036A CN 201010277903 A CN201010277903 A CN 201010277903A CN 101962425 B CN101962425 B CN 101962425B
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- 125000000129 anionic group Chemical group 0.000 title claims abstract description 34
- 239000010813 municipal solid waste Substances 0.000 title claims abstract description 29
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000003999 initiator Substances 0.000 claims abstract description 22
- 125000002091 cationic group Chemical group 0.000 claims abstract description 20
- 230000014759 maintenance of location Effects 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 150000004820 halides Chemical class 0.000 claims abstract description 10
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920000962 poly(amidoamine) Polymers 0.000 claims abstract 11
- 238000006243 chemical reaction Methods 0.000 claims description 42
- 239000000126 substance Substances 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- -1 carboxylic acid halides Chemical class 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 150000002500 ions Chemical class 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- 241000555268 Dendroides Species 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 230000000694 effects Effects 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000010008 shearing Methods 0.000 claims description 10
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 230000001143 conditioned effect Effects 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- 125000000524 functional group Chemical group 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 5
- 229920006317 cationic polymer Polymers 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 claims description 4
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000005457 ice water Substances 0.000 claims description 4
- 239000012044 organic layer Substances 0.000 claims description 4
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- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- LSTRKXWIZZZYAS-UHFFFAOYSA-N 2-bromoacetyl bromide Chemical compound BrCC(Br)=O LSTRKXWIZZZYAS-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000011859 microparticle Substances 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- VGCXGMAHQTYDJK-UHFFFAOYSA-N Chloroacetyl chloride Chemical compound ClCC(Cl)=O VGCXGMAHQTYDJK-UHFFFAOYSA-N 0.000 claims description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical group [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 2
- 229940045803 cuprous chloride Drugs 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 abstract description 17
- 238000010560 atom transfer radical polymerization reaction Methods 0.000 abstract description 6
- 230000000977 initiatory effect Effects 0.000 abstract description 4
- 125000003277 amino group Chemical group 0.000 abstract description 2
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
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- 239000008107 starch Substances 0.000 description 3
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- 238000010521 absorption reaction Methods 0.000 description 2
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- 238000013019 agitation Methods 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 241000274582 Pycnanthus angolensis Species 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 description 1
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- 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
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a dendrimer-star anionic trash catcher, which is a cationic dendrimer-star polymer with 4 to 256 branched arms, molecular weight of 1,000 to 1,000,000 and cationic charge density of 1 to 10 meq.g<-1>. In N,N-dimethylformamide, the terminal amino group of the entire dendrimer polyamidoamine is modified by acyl halide to prepare a dendrimer macromolecular polyfunctional initiator; and atom transfer radical polymerization initiating a quaternary ammonium cationic monomer is realized by taking the initiator as an initiation start core, cuprous halide as a catalyst and 2,2'-bipyridyl as a ligand. Before paper retention and filter aid is used, the cationic dendrimer-star polymer is added into a paper material and used as the anionic trash catcher, and the wet papermaking system can be optimized and the paper quality can be improved.
Description
Technical field
The present invention relates to a kind of tree nuclear star shape polymer anion rubbish trapping agent, belong to pulping and paper-making industry wet-end chemicals technical field.
Background technology
Along with the adjustment (as a large amount of uses of paper waste, high yield pulp) of paper industry raw material mix, the raising of paper machine white water system lock circulation degree and the use of various papermaking chemical products, the manufacture paper with pulp aggregation extent and the concentration of the interference anionic impurity (anionic trash) in the system of wet end of machine is more and more higher.They can act on cationic chemical auxiliary agent (as dried Wet Strength Resin, retention filtration adjuvant etc.), reduce their action effect; Or form agglomerate and be deposited on wire-cloth, felt, vacuum furnace, suction box, drying cylinder etc. and locate, reduce paper machine behaviour in service; Perhaps be adsorbed on fiber, the fiber fines, reduce interfibrous hydrogen bonded, influence into the strength property of paper.Improve paper machine speed in order to strengthen the paper stock drainage, what increase fiber fines and filler etc. keeps the minimizing wasting of resources, improve paper-forming evenness and improve page characteristic, improve whitewater closure circulation degree and stable paper machine operation, just need use anionic trash trapping agent (anionic trash catcher) efficiently, eliminate or the prevention anionic trash to the manufacture paper with pulp harm of system of wet end of machine.
At present both at home and abroad the anionic trash trapping agent that adopts is generally Gaoyang electric density, low-molecular-weight linearity or branched polymer, as the cationic starch of polyamine, polymine and modifier thereof, diallyl dimethyl ammoniumchloride, cationic polyacrylamide, high substitution value etc.They can in and dissolved anionic species in the paper stock, or the colloid anionic impurity is fixed on paper pulp fiber or the filler with condensation mechanism, take out of with page and copy paper system, reach the purpose of cleaning system.
But the molecular chain form of polymkeric substance has very big influence to its action effect.In use, effects such as the polymer molecule of linear structure can adsorb on paper stock component surface, reconstruct and diffusion, reduction result of use.Especially in the high system of whitewater closure circulation degree, constantly the water-soluble inorganic salt that accumulates will cause system's specific conductivity to rise, and the polymer molecular chain of linear structure can shrink and curl under the high conductivity condition, to the ability to function reduction of electronegative material.And the molecular chain of star polymer be because the repulsive interaction between each arm can be taked the conformation that more stretches, and the wadding cumulative power of building bridge is strong, has than the better action effect of linear polymer.Li etc. studies show that, positively charged ion star polymer and high molecular with 21 branching arms, the double base wadding aggressiveness system that the anionic polymer of low charge density is formed has the poly-effect of extraordinary wadding to china clay, and this double element system can also improve the removal efficient of fats component, referring to Li J, Modak P R, Xiao H.Novelflocculation system based on 21-arm cationic star polymer[J] .Colloids and Surface A:Physicochemical and Engineering Aspects, 2006,289 (1-3): 172-178.
Along with the development of polymer science, particularly continuous understanding to concerning between macromolecular structure and performance, every field is more and more paid attention to the research and development of highly-branched polymers.The synthetic polymer that improves performance, the development of new highly branched structure of conventional linear or branched polymer paper making additive becomes the target that paper industry is pursued.It is peripheral and tree nuclear star shape polymkeric substance that form has caused people's common concern with its particular structure and performance to receive dendritic macromole by many linear side chains with chemical bond-linking.Synthetic can the employing with the dendroid multifunctional initiator of tree nuclear star shape polymkeric substance is that centronucleus, trigger monomer polymerization formation structure are determined macromolecular " examining postbrachium earlier " method (Core first) and will be synthesized good linear polymer and " examining behind the first arm " method (Arm first) of dendroid polyfunctional group coupling agent coupling in advance.Two kinds of approach all can synthesize the have controlled architecture tree nuclear star shape polymkeric substance of (branching arm number, brachium, sequential structure).And atom transfer radical polymerization (ATRP) with the molecular structure and the molecular-weight average of its synthetic polymer can control, the equal first-class characteristics of each branching arm chain length, become the tree nuclear star shape synthetic method of polymers that has development prospect.Liu Hu etc. with bromoacetyl bromide to the 4.0th generation polypropylene imines dendritic macromole carry out modification, successfully synthesized dendritic macromole initiator DAB-32-Br, be catalyst/initiator system then with DAB-32-Br/CuBr/Bpy, in Shui Heshui/ethanol medium, realized the atom transfer radical polymerization of N-N-isopropylacrylamide respectively, referring to Liu Hu, Zhu Yanjin, Yi Changfeng, Deng. the preparation [J] of dendritic macromole/poly-(N-N-isopropylacrylamide) nanoparticle. the process engineering journal, 2008,8 (6): 1245-1248.
Dendroid polyamide-amide (PAMAM) is to study maximum dendritic macromoles at present.Its molecular structure is highly branched, and has the geometrical symmetry of height, and there is cavity in intramolecule, and the surface has very high functional group densities.Introducing suitable active function group in its molecular end, is the atom transfer radical polymerization of branching core trigger monomer with the dendroid multifunctional initiator that generates again, can the composite structure novelty, the tree nuclear star shape polymkeric substance of the narrow distribution of molecular weight.With the dendroid polyamide-amide is that the tree nuclear star shape polymkeric substance of initial core has more wide development and application prospect as a kind of polymer with novel structure, form and function.
Summary of the invention
At the deficiencies in the prior art, and, the invention provides a kind of positively charged ion tree nuclear star shape anionic trash trapping agent and application thereof in conjunction with paper making wet part the manufacture paper with pulp characteristics and the requirement of system.
Summary of the invention
The present invention sets nuclear star shape anionic trash trapping agent and prepares in two steps, the one, at N, in the N dimethyl formamide (DMF), adopt carboxylic acid halides to modify for the terminal amino group of dendroid polyamide-amide (Gn.0PAMAM), make dendritic macromole multifunctional initiator (Gn.0PAMAM-X) whole; The 2nd, serve as that the initial core of initiation, cuprous halide are catalyzer, 2 with this dendritic macromole multifunctional initiator (Gn.0PAMAM-X), 2 '-dipyridyl is a part, cause the monomeric atom transfer radical polymerization of quaternary ammonium cation, synthesizing cationic tree nuclear star shape polymkeric substance, promptly.
The term explanation:
Whole for the dendroid polyamide-amide, note by abridging and be Gn.0PAMAM;
Hold amino number be respectively 4,8,16,32,64,128,256 the 1.0th, 2.0,3.0,4.0,5.0,6.0,7.0 generation the dendroid polyamide-amide, brief note is G1.0PAMAM, G2.0PAMAM, G3.0PAMAM, G4.0PAMAM, G5.0PAMAM, G6.0PAMAM, G7.0PAMAM respectively;
The dendritic macromole multifunctional initiator is noted by abridging and is Gn.0PAMAM-X, and X represents Cl or Br.
Detailed Description Of The Invention
Technical scheme of the present invention is as follows:
A kind of tree nuclear star shape anionic trash trapping agent is that branching arm number is 4～256, molecular weight is 1000～1000000, cationic charge density is 1～10meqg
-1Positively charged ion tree nuclear star shape polymkeric substance, make according to following steps:
1, at ice-water bath and under stirring, in advance carboxylic acid halides is dissolved in N, in the N dimethyl formamide (DMF), is mixed with the DMF solution of carboxylic acid halides, airtight preservation is standby down at 0～5 ℃.Then; in reactor, add N; N dimethyl formamide (DMF); whole to wherein dripping under stirring and high pure nitrogen protection for dendroid polyamide-amide (Gn.0PAMAM) and acid binding agent; the temperature that mixes in the conditioned reaction device of back is 0～5 ℃, then to the slow DMF solution of the carboxylic acid halides for preparing in advance of dropping wherein.Drip the back and react 1～12h down at 0～5 ℃, the temperature in the conditioned reaction device is 5-50 ℃ then, continues reaction 1～48h again.After reaction is finished the reaction solution underpressure distillation removed and desolvate, be dissolved in the chloroform again, and use the aqueous hydrochloric acid of 10wt%, saturated aqueous sodium carbonate and deionized water wash respectively, the organic layer underpressure distillation of telling removes and desolvates, and promptly gets dendritic macromole multifunctional initiator (Gn.0PAMAM-X) after vacuum-drying.
Above-mentioned carboxylic acid halides is one of 2-bromo isobutyl acylbromide, bromoacetyl bromide or chloroacetyl chloride.
Above-mentioned putting in order is selected from one of G1.0PAMAM, G2.0PAMAM, G3.0PAMAM, G4.0PAMAM, G5.0PAMAM, G6.0PAMAM or G7.0PAMAM for dendroid polyamide-amide (Gn.0PAMAM).
2, in reactor, add alcohol-water solution, stirring and feeding dendritic macromole multifunctional initiator (Gn.0PAMAM-X) and the quaternary ammonium cation monomer that adding step 1 makes under the nitrogen then.After reaction monomers mixes, be warming up to 25～100 ℃ of temperature of reaction, under nitrogen protection, add cuprous halide and 2,2 '-dipyridyl.Regulating the quaternary ammonium cation monomer concentration is 1～50wt%, isothermal reaction 1～48h.Reaction solution is cooled to room temperature, and filters, in filtrate, add acetone then product is precipitated out, and be drying to obtain positively charged ion tree nuclear star shape polymkeric substance through the acetone washing by soaking and under vacuum through alumina column.
Preferably, in the above-mentioned steps 1:
Described acid binding agent is one of triethylamine, tripropyl amine or pyridine.
In the described reaction system, carboxylic acid halides is (1～10) with whole mol ratio for dendroid polyamide-amide (Gn.0PAMAM) end amino: 1.
In the described reaction system, the mol ratio of acid binding agent and carboxylic acid halides is (0.1～1): 1.
It is 4,8,16,32,64,128,256 G1.0PAMAM-Br or G1.0PAMAM-Cl, G2.0PAMAM-Br or G2.0PAMAM-Cl, G3.0PAMAM-Br or G3.0PAMAM-Cl, G4.0PAMAM-Br or G4.0PAMAM-Cl, G5.0PAMAM-Br or G5.0PAMAM-Cl, G6.0PAMAM-Br or G6.0PAMAM-Cl, G7.0PAMAM-Br or G7.0PAMAM-Cl that the dendritic macromole multifunctional initiator (Gn.0PAMAM-X) that described reaction obtains is respectively end functional group number.As the initial core of the initiation of step 2.
Preferably, in the above-mentioned steps 2:
Alcohol in the described alcohol-water solution is ethanol, 2-propyl alcohol or propyl alcohol; The alcohol in the described alcohol-water solution and the volume ratio of water are (0.1～10): 1.Described water is deionized water.
Described cuprous halide is cuprous chloride or cuprous bromide.
Described quaternary ammonium cation monomer is acrylyl oxy-ethyl-trimethyl salmiac (AETMAC), methylacryoyloxyethyl trimethyl ammonium chloride (DMC) or dimethyl diallyl ammonium chloride (DADMAC).
In the described reaction system, the mol ratio of the end functional group of quaternary ammonium cation monomer and dendritic macromole multifunctional initiator (Gn.0PAMAM-X) is (1～500): 1; The mol ratio of the end functional group of cuprous halide and dendritic macromole multifunctional initiator (Gn.0PAMAM-X) is (1～5): 1; Cuprous halide and 2, the mol ratio of 2 '-dipyridyl are 1: (1～10).
The tree nuclear star shape polymkeric substance that the reaction of the above method of the present invention obtains is that branching arm number is 4～256, molecular weight is 1000～1000000, cationic charge density is 1～10meqg
-1Positively charged ion tree nuclear star shape polymkeric substance; As manufacture paper with pulp anionic trash trapping agent in the system of paper making wet part.
The application of tree nuclear star shape anionic trash trapping agent of the present invention is that above-mentioned gained positively charged ion tree nuclear star shape polymkeric substance was added in the paper stock before using paper retention and filter aid.Method is as follows, and following per-cent all is the weight percents to the over dry paper stock:
Being added with concentration that 0%～50% filler, 0.1%～2% sizing agent be mixed with is in 0.5%～5% the paper stock, adds 0.01%～5% positively charged ion tree nuclear star shape polymkeric substance, and thorough mixing is even.Behind 1min～2h, continue one of following steps:
(1) the high-molecular cationic polymer paper retention and filter aid of adding 0.01%～1% is copied into paper behind effect 10s～30min; Perhaps
(2) the high-molecular cationic polymer paper retention and filter aid of adding 0.01%～1%, improve the shearing force of paper stock system behind effect 60s～5min, recover the shearing force level of paper stock system behind maintenance 60s～10min, add 0.1%～1% anionic microparticles again, copy into paper behind effect 10s～30min.
In order to the paper that last method is copied, the retention of paper stock can reach more than 90%, and the quickening of the drainage rate of paper stock, and paper machine operation is stable.White water consistency and anionic trash content wherein reduce greatly.
Above-mentioned filler is selected from precipitated chalk, grinding calcium carbonate or talcum powder.
Above-mentioned sizing agent is selected from gum rosin, alkyl ketene dimer (AKD) or alkenyl succinic anhydride (ASA).
Above-mentioned high-molecular cationic polymer paper retention and filter aid is selected from cationic polyacrylamide, cationic starch, cationic polyacrylamide graft starch one of them or combination.
Above-mentioned anionic microparticles is meant wilkinite, colloid silica, the little polymers of organic anion one of them or combination.
Above-mentioned paper stock is meant paper waste (OCC, ONP), mechanical pulp, high yield pulp (APMP, BCTMP) one of them or wherein several mixed pulp.
The regular compactness of molecular structure, segment density height, the stretching, extension of molecular chain conformation, positive charge density height, the soltion viscosity of positively charged ion tree nuclear star shape polymkeric substance of the present invention are low, strong with the ability to function of anionic trash.With paper making wet part retention filtration adjuvant synergy, can in the retention that improves tiny component, the drainage rate of quickening paper stock, improve paper quality at web part of paper machine.And machine water concentration is reduced, and reduce of the harm of negatively charged ion objectionable impurities to the paper production process, guarantee the normal operation of paper machine.
Description of drawings
Fig. 1 is the schematic arrangement of the positively charged ion tree nuclear star shape polymkeric substance of the embodiment of the invention 1.
Embodiment
The invention will be further described below in conjunction with embodiment.Except that specifying, the per-cent among the embodiment all is weight percentage.The water of using in step among the embodiment (2) ethanol-water solution is deionized water, specific conductivity 2～4uscm
-1
Embodiment 1:
(1) under ice-water bath and magnetic agitation, in advance 13.79g 2-bromo isobutyl acylbromide is dissolved in 55mL N, in the N dimethyl formamide (DMF), wiring solution-forming.In the reactor that constant voltage feeding device, reflux condensate device (connect gas absorbing device on the reflux condensing tube, with rare NaOH liquid as gas absorption liquid), temperature adjustment and whipping appts are housed, add 45mLDMF.Temperature in the controlling reactor drips 7.15g the 2.0th generation dendroid polyamide-amide (G2.0PAMAM) and 4.45g triethylamine below 5 ℃ successively at feeding nitrogen and under stirring.Mix the back to the slow DMF solution of the 2-bromo isobutyl acylbromide for preparing in advance of dropping wherein.Be added dropwise to complete the back and react 12h down at 0～5 ℃, the temperature in the conditioned reaction device is 25 ℃ then, continues reaction 24h again.The reaction solution underpressure distillation removed desolvate, be dissolved in the chloroform again, and use the aqueous hydrochloric acid of 10wt%, saturated aqueous sodium carbonate and deionized water wash respectively, telling organic layer removes through underpressure distillation and desolvates, after vacuum-drying, promptly getting and holding functional group's number is 8 dendritic macromole multifunctional initiator G2.0PAMAM-Br.
(2) in the reactor that thermometer, reflux condensate device, nitrogen turnover pipe, magnetic stirring apparatus and register are housed, the dendritic macromole multifunctional initiator G2.0PAMAM-Br 1.3g that adding prepares in advance and the ethanol-water solution (volume ratio of alcohol to water is 1: 1) of 99.4g acrylyl oxy-ethyl-trimethyl salmiac.Feed the nitrogen deoxygenation, mix the temperature in the conditioned reaction device of back.When temperature of reaction system rises to 70 ℃, under nitrogen protection, add 1.15g cuprous bromide and 2.5g 2,2 '-dipyridyl.Regulating total monomer concentration is 15%.Isothermal reaction 12h.Reaction solution is cooled to room temperature, and filters, in filtrate, add acetone then product is precipitated out,, promptly get positively charged ion tree nuclear star shape polymkeric substance through acetone washing by soaking and dry under vacuum through alumina column.
The branching arm number of gained tree nuclear star shape polymkeric substance is 8, molecular weight is 100,000～150,000, cationic charge density is 5.1meqg
-1
As follows as the paper making wet part application of anionic trash trapping agent of manufacturing paper with pulp in the system:
The bleaching crushed news deinking slurry that has added the AKD sizing agent of 20% precipitated chalk and 1% is deployed into 0.5% concentration, the positively charged ion tree nuclear star shape polymkeric substance that above-mentioned steps with 0.1% (2) makes joins in the slurry system, behind the reaction 5min, add 0.05% cationic polyacrylamide.Behind the effect 60s paper stock is copied into paper, the retention of dry back paper stock can reach 91%, and the paper stock drainage rate is accelerated, and white water consistency reduces greatly.
Embodiment 2: as embodiment 1, and when different is application,
The slurry of APMP slurry (alkaline peroxide mechanical pulp) allotment to 0.5% of AKD sizing agent that has added 25% lime carbonate and 1% is dense, the positively charged ion tree nuclear star shape polymkeric substance that embodiment 1 step (2) with 0.1% makes joins in the slurry system, behind the effect 5min, add 0.05% cationic polyacrylamide.Improve the shearing force of paper stock system behind the 60s, recover the shearing force of paper stock system behind the 120s, add 0.45% colloid silica.Behind the effect 60s paper stock is copied into paper, the retention of dry back paper stock can reach 92%, and the paper stock drainage rate is accelerated, and white water consistency reduces greatly, and quality of finished paper is improved.
Embodiment 3:
(1) under ice-water bath and magnetic agitation, in advance 13.8g 2-bromo isobutyl acylbromide is dissolved in 60mL N, in the N dimethyl formamide (DMF), be mixed with solution.In the reactor that constant voltage feeding device, reflux condensate device (connect gas absorbing device on the reflux condensing tube, with rare NaOH liquid as gas absorption liquid), temperature adjustment and whipping appts are housed, add 50mL DMF.Temperature in the controlling reactor drips 8.1g the 3.0th generation dendroid polyamide-amide (G3.0PAMAM) and 4.86g triethylamine below 5 ℃ successively at feeding nitrogen and under stirring.Mix the back to the slow DMF solution of the 2-bromo isobutyl acylbromide for preparing in advance of dropping wherein.Be added dropwise to complete the back and react 12h down at 0～5 ℃, the temperature in the conditioned reaction device is 30 ℃ then, continues reaction 36h again.The reaction solution underpressure distillation removed desolvate, be dissolved in the chloroform again, and use the aqueous hydrochloric acid of 10wt%, saturated aqueous sodium carbonate and deionized water wash respectively, telling organic layer removes through underpressure distillation and desolvates, after vacuum-drying, promptly getting and holding functional group's number is 16 dendritic macromole multifunctional initiator G3.0PAMAM-Br.
(2) in the reactor that thermometer, reflux condensate device, nitrogen turnover pipe, magnetic stirring apparatus and register are housed, the 2.82g dendroid multifunctional initiator G3.0PAMAM-Br that adding prepares in advance and the ethanol-water solution (volume ratio of alcohol to water is 1: 1) of 154.94g acrylyl oxy-ethyl-trimethyl salmiac.Feed the nitrogen deoxygenation, mix the temperature in the conditioned reaction device of back.When temperature of reaction system rises to 75 ℃, under nitrogen protection, add 2.3g cuprous bromide and 5g 2,2 '-dipyridyl.Regulating total monomer concentration is 15%.Isothermal reaction 24h.Reaction solution is cooled to room temperature, and filter through alumina column, in filtrate, add acetone then product is precipitated out, through acetone washing by soaking and dry under vacuum, promptly get branching arm number and be 16, molecular weight is 200,000～250,000, cationic charge density is 5.0meqg
-1Positively charged ion tree nuclear star shape polymkeric substance.
As follows as the paper making wet part application of anionic trash trapping agent of manufacturing paper with pulp in the system:
The slurry of BCTMP slurry (bleached chemical thermomechanical pulp) allotment to 0.5% of AKD sizing agent that has added 20% lime carbonate and 1% is dense, the positively charged ion tree nuclear star shape polymkeric substance that above-mentioned steps with 0.1% (2) makes joins in the slurry system, behind the effect 10min, add 0.05% cationic polyacrylamide.Improve the shearing force of paper stock system behind the 60s, recover the shearing force of paper stock system behind the 120s, add 0.45% colloid silica.Behind the effect 60s paper stock is copied into paper, the retention of dry back paper stock can reach 92.5%, and the paper stock drainage rate is accelerated, and white water consistency reduces greatly, and quality of finished paper is improved.
Embodiment 4: as embodiment 1, different is that applied slurry is the BCTMP slurry.
Embodiment 5: as embodiment 1, different is that applied slurry is the APMP slurry.
Embodiment 6: as embodiment 2, different is that the filler of using is a talcum powder, and the pH value that adds Tai-Ace S 150 adjusting paper stock is 5-7.Behind the cationic polyacrylamide of adding 0.05%, improve the shearing force of paper stock system, reduce the shearing force of paper stock system then, add 0.4% wilkinite.
Embodiment 7: as embodiment 1, different is that applied slurry is useless boxboard paper pulp.
Embodiment 8: as embodiment 3, different is that applied slurry is bleaching crushed news deinking slurry.
Claims (10)
1. tree nuclear star shape anionic trash trapping agent is that branching arm number is 4～256, molecular weight is 1000～1000000, cationic charge density is 1～10meqg
-1Positively charged ion tree nuclear star shape polymkeric substance, make according to the following steps:
(1) at ice-water bath and under stirring, carboxylic acid halides is dissolved in N, in the N dimethyl formamide (DMF), is mixed with the DMF solution of carboxylic acid halides, airtight preservation is standby down at 0～5 ℃;
Then, in reactor, add N, N dimethyl formamide (DMF), whole to wherein dripping under stirring and high pure nitrogen protection for dendroid polyamide-amide (Gn.0 PAMAM) and acid binding agent, the temperature that mixes in the conditioned reaction device of back is 0～5 ℃, to the DMF solution that wherein drips the carboxylic acid halides for preparing in advance, drips back reaction 1～12h under 0～5 ℃, temperature in the conditioned reaction device is 5-50 ℃ then, continues reaction 1～48h again;
After reaction is finished, the reaction solution underpressure distillation removed desolvate, be dissolved in the chloroform again, and use the aqueous hydrochloric acid of 10wt%, saturated aqueous sodium carbonate and deionized water wash respectively, the organic layer underpressure distillation of telling removes and desolvates, and promptly gets dendritic macromole multifunctional initiator (Gn.0 PAMAM-X) after vacuum-drying;
Described carboxylic acid halides is 2-bromo isobutyl acylbromide, bromoacetyl bromide or chloroacetyl chloride;
Described putting in order is selected from G1.0 PAMAM, G2.0 PAMAM, G3.0 PAMAM, G4.0 PAMAM, G5.0 PAMAM, G6.0 PAMAM or G7.0 PAMAM for dendroid polyamide-amide (Gn.0 PAMAM);
(2) in reactor, add alcohol-water solution, under stirring and feeding nitrogen, add dendritic macromole multifunctional initiator (Gn.0 PAMAM-X) and the quaternary ammonium cation monomer that step (1) makes then, be warming up to 25～100 ℃ of temperature of reaction after mixing, under nitrogen protection, add cuprous halide and 2,2 '-dipyridyl, regulating the quaternary ammonium cation monomer concentration is 1～50wt%, isothermal reaction 1～48h;
Then, reaction solution is cooled to room temperature, and filters, in filtrate, add acetone product is precipitated out, be drying to obtain positively charged ion tree nuclear star shape polymkeric substance through the acetone washing by soaking and under vacuum through alumina column.
2. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that acid binding agent is one of triethylamine, tripropyl amine or pyridine described in the step (1).
3. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that in step (1) reaction system, and carboxylic acid halides is (1～10) with whole mol ratio for dendroid polyamide-amide (Gn.0 PAMAM) end amino: 1.
4. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that the mol ratio of acid binding agent and carboxylic acid halides is (0.1～1): 1 in step (1) reaction system.
5. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that the alcohol in the alcohol-water solution is ethanol or propyl alcohol described in the step (2).
6. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that cuprous halide is cuprous chloride or cuprous bromide described in the step (2).
7. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that quaternary ammonium cation monomer described in the step (2) is acrylyl oxy-ethyl-trimethyl salmiac (AETMAC), methylacryoyloxyethyl trimethyl ammonium chloride (DMC) or dimethyl diallyl ammonium chloride (DADMAC).
8. tree nuclear star shape anionic trash trapping agent as claimed in claim 1, it is characterized in that in step (2) reaction system, the mol ratio of the end functional group of quaternary ammonium cation monomer and dendritic macromole multifunctional initiator (Gn.0 PAMAM-X) is (1～500): 1; The mol ratio of the end functional group of cuprous halide and dendritic macromole multifunctional initiator (Gn.0 PAMAM-X) is (1～5): 1.
9. tree nuclear star shape anionic trash trapping agent as claimed in claim 1 is characterized in that in step (2) reaction system, cuprous halide and 2, and the mol ratio of 2 '-dipyridyl is 1: (1～10).
10. the application of the described tree nuclear star of claim 1 shape anionic trash trapping agent is that described positively charged ion tree nuclear star shape polymkeric substance was added in the paper stock before using paper retention and filter aid, and method is as follows, and following per-cent all is the weight percents to the over dry paper stock:
In the paper stock that is added with the concentration 0.5%～5% that 0%～50% filler, 0.1%～2% sizing agent be mixed with, add 0.01%～5% positively charged ion tree nuclear star shape polymkeric substance, mix; Behind 1min～2h, continue one of following steps:
(1) the high-molecular cationic polymer paper retention and filter aid of adding 0.01%～1% is copied into paper behind effect 10s～30min; Perhaps
(2) the high-molecular cationic polymer paper retention and filter aid of adding 0.01%～1%, improve the shearing force of paper stock system behind effect 60s～5min, recover the shearing force level of paper stock system behind maintenance 60s～10min, add 0.1%～1% anionic microparticles again, copy into paper behind effect 10s～30min.
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| CN104420382B (en) * | 2013-08-28 | 2016-08-17 | 天津科技大学 | Containing anionic trash control method in high yield pulp mixed slurry |
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| CN109181659A (en) * | 2018-09-10 | 2019-01-11 | 长江大学 | End group is the dendrimer intercalator and preparation method thereof of quaternary ammonium group |
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| CN101818464A (en) * | 2010-03-16 | 2010-09-01 | 华泰集团有限公司 | Multi-arm branched cationic polymer retention and drainage aid for papermaking, and preparation method and application thereof |
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| CN101818464A (en) * | 2010-03-16 | 2010-09-01 | 华泰集团有限公司 | Multi-arm branched cationic polymer retention and drainage aid for papermaking, and preparation method and application thereof |
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