CN114292406B - Preparation method of wrinkling cylinder sticking agent - Google Patents
Preparation method of wrinkling cylinder sticking agent Download PDFInfo
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- CN114292406B CN114292406B CN202111632039.1A CN202111632039A CN114292406B CN 114292406 B CN114292406 B CN 114292406B CN 202111632039 A CN202111632039 A CN 202111632039A CN 114292406 B CN114292406 B CN 114292406B
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- 238000002360 preparation method Methods 0.000 title abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229920000642 polymer Polymers 0.000 claims abstract description 72
- 239000004952 Polyamide Substances 0.000 claims abstract description 37
- 229920002647 polyamide Polymers 0.000 claims abstract description 37
- 229920000768 polyamine Polymers 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000853 adhesive Substances 0.000 claims abstract description 13
- 230000001070 adhesive effect Effects 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims description 77
- 239000000243 solution Substances 0.000 claims description 65
- 239000007787 solid Substances 0.000 claims description 46
- 238000003756 stirring Methods 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 28
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims description 24
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 239000000376 reactant Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 230000000844 anti-bacterial effect Effects 0.000 claims description 12
- 239000003899 bactericide agent Substances 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 12
- 239000001361 adipic acid Substances 0.000 claims description 11
- 235000011037 adipic acid Nutrition 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 claims description 10
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 10
- 238000010790 dilution Methods 0.000 claims description 10
- 239000012895 dilution Substances 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 10
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 9
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 9
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 7
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- 229960001124 trientine Drugs 0.000 claims description 6
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 5
- 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 5
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 5
- UZNHKBFIBYXPDV-UHFFFAOYSA-N trimethyl-[3-(2-methylprop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)NCCC[N+](C)(C)C UZNHKBFIBYXPDV-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims 4
- 239000000178 monomer Substances 0.000 abstract description 46
- 239000004593 Epoxy Substances 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011203 carbon fibre reinforced carbon Substances 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 238000010526 radical polymerization reaction Methods 0.000 abstract description 3
- 125000003700 epoxy group Chemical group 0.000 abstract 1
- 238000007142 ring opening reaction Methods 0.000 abstract 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 abstract 1
- 239000000047 product Substances 0.000 description 27
- 239000000203 mixture Substances 0.000 description 11
- 125000002091 cationic group Chemical group 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 5
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 4
- 239000002738 chelating agent Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012986 chain transfer agent Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 2
- -1 polyoxyethylene Polymers 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 description 1
- KTLIZDDPOZZHCD-UHFFFAOYSA-N 3-(2-aminoethylamino)propan-1-ol Chemical compound NCCNCCCO KTLIZDDPOZZHCD-UHFFFAOYSA-N 0.000 description 1
- MTEXJGQBDXDJRH-UHFFFAOYSA-N 3-[amino(ethyl)amino]propan-1-amine Chemical compound CCN(N)CCCN MTEXJGQBDXDJRH-UHFFFAOYSA-N 0.000 description 1
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 1
- STHWVYJPPPDLSL-UHFFFAOYSA-N CC(C)CCCC(C)OC(=O)C=C Chemical compound CC(C)CCCC(C)OC(=O)C=C STHWVYJPPPDLSL-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- LHIJANUOQQMGNT-UHFFFAOYSA-N aminoethylethanolamine Chemical compound NCCNCCO LHIJANUOQQMGNT-UHFFFAOYSA-N 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- UUORTJUPDJJXST-UHFFFAOYSA-N n-(2-hydroxyethyl)prop-2-enamide Chemical compound OCCNC(=O)C=C UUORTJUPDJJXST-UHFFFAOYSA-N 0.000 description 1
- YPHQUSNPXDGUHL-UHFFFAOYSA-N n-methylprop-2-enamide Chemical compound CNC(=O)C=C YPHQUSNPXDGUHL-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000962 poly(amidoamine) Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003335 secondary amines Chemical group 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 1
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- Polyamides (AREA)
- Paper (AREA)
Abstract
The invention discloses a preparation method of wrinkling cylinder sticking agent, belonging to the field of papermaking, comprising preparation of a polymer A containing epoxy end groups containing carbon-carbon double bonds, acrylamide groups, flexible groups and quaternary ammonium salt cationic groups; preparing a polyamide polyamine polymer B; the epoxy groups in the polymer A and the secondary amine groups in the polymer B are subjected to ring opening reaction; and adjusting auxiliary parameters. The invention obtains the cylinder adhesive product by further reacting the polymer obtained by free radical polymerization of epoxy end group monomer containing carbon-carbon double bond, acrylamide monomer, flexible monomer and quaternary ammonium salt cationic monomer with polyamide polyamine polymer. The defect that a single PAE resin wrinkling coating becomes hard and brittle at high temperature can be effectively overcome, so that the adhesive force, film forming property and water resistance of the product are improved to a higher level, and the product can be suitable for toilet paper machines with different configuration levels and various household papers for producing different paper types.
Description
Technical Field
The invention belongs to the field of papermaking, and in particular relates to a preparation method of wrinkling cylinder sticking agent.
Background
One type of cylinder sticking agent currently used in the market is polyamide polyamine-epichlorohydrin resin, namely PAE resin, and the type of cylinder sticking agent can form a hard water-resistant coating film on a drying cylinder. However, since the degree of crosslinking of epichlorohydrin and polyamide has a great influence on the rewettability and the adhesion of PAE resin, the properties thereof are difficult to change in a given creping process, and when the water content of the paper web is low or the temperature of the drying cylinder is too high, the PAE resin on the surface of the drying cylinder becomes hard and brittle, thereby causing the adhesion to decrease, deteriorating the creping effect, and failing to well meet the requirements of different household paper products or different paper machines for the coating.
Many researchers have synthesized other agents such as polyacrylamide-dimethylallyl ammonium chloride copolymer cylinder sticking agents, polyethylene imine cylinder sticking agents, polyvinyl alcohol cylinder sticking agents, which can solve some problems in the paper wrinkling process, but have the following drawbacks: 1. although the phenomena of paper tearing and uneven wrinkling in the paper wrinkling process are improved, the problem of poor film forming property is not solved; 2. the polyethyleneimine is difficult to synthesize, and the product price is high; 3. the addition of the flexible monomer and the plasticizer to the synthesized polyacrylamide-based cylinder sticking agent improves the film forming property and rewettability of the product, but reduces the adhesive force of the product.
Disclosure of Invention
In order to overcome the technical defects, the invention provides a preparation method of wrinkling cylinder sticking agent, which aims to solve the problems related to the background technology.
The invention provides a preparation method of wrinkling cylinder sticking agent, which comprises the following steps:
adding water, epoxy end group monomers containing carbon-carbon double bonds, acrylamide monomers, flexible monomers and cationic monomers into a reaction bottle, regulating the pH of the solution to 3.5-4.5, adding a chelating agent and a chain transfer agent, introducing nitrogen to remove oxygen, then slowly heating to 70 ℃, slowly dropwise adding ammonium persulfate solution initiator and part of acrylamide monomers, keeping the temperature at 75-85 ℃ for 4 hours after the dropwise adding is finished, stopping heating, adding water to regulate the solid content to 10-20wt%, and cooling to room temperature to obtain a polymer A solution;
after the polybasic organic amine and the dibasic organic carboxylic acid react for 1-8 hours at 140-180 ℃, adding water accounting for 80% -90% of the total mass of the organic amine and the organic carboxylic acid, and obtaining a polyamide polyamine polymer B solution;
uniformly mixing the polymer A and the polymer B, then reacting for 1-5 hours at 40-80 ℃, and adding water to terminate the reaction when the solution viscosity reaches 250-400mPa.s to obtain a reactant;
cooling the reactant to 30-35 ℃, adding 32% liquid alkali to adjust the pH value of the solution to 8-10, then adding a bactericide, and uniformly stirring to obtain a cylinder sticking agent; the viscosity of the product is controlled to be 30-250mPa.s, and the solid content is controlled to be 10-20wt%.
Preferably or optionally, the epoxy end group monomer containing carbon-carbon double bonds is one or more of glycidyl ether allyl alcohol polyoxyethylene ether, allyl Glycidyl Ether (AGE), glycidyl Acrylate (GA) and Glycidyl Methacrylate (GMA);
the mass of the epoxy end group monomer containing carbon-carbon double bonds is 10-50% of the total mass of the polymer monomer.
Preferably or alternatively, the glycidyl ether allyl alcohol polyoxyethylene ether has the following structure:
wherein q is more than or equal to 9 and less than or equal to 15.
Preferably or optionally, the acrylamide monomer is selected from one or more of acrylamide, N-methylacrylamide, N-dimethylacrylamide, N-diethylacrylamide, N-methylolacrylamide and N-hydroxyethyl acrylamide;
the mass of the acrylamide monomer is 50% -80% of the total mass of the polymer monomer.
Preferably or optionally, the flexible monomer is one or more of methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, n-octyl acrylate, 2-isooctyl acrylate, 2-hydroxyethyl acrylate and 2-hydroxypropyl acrylate;
the mass of the flexible monomer is 1% -45% of the total mass of the polymer monomer.
Preferably or alternatively, the cationic monomer is selected from one or more of (meth) acryloyloxyethyl trimethyl ammonium chloride (DMC or DAC), methacrylamidopropyl trimethyl ammonium chloride (PMC), dimethyl diallyl ammonium chloride (DMDAAC);
the mass of the cationic monomer is 1% -45% of the total mass of the polymer monomer.
Preferably or alternatively, the chelating agent is one of the chelating agents EDTA-2Na or DTPA-Na 5;
the mass fraction of the chelating agent in the polymer solution is 0.003% -0.02%.
The chain transfer agent is one or more of sodium hypophosphite, isopropanol, sodium formate, thioglycollic acid and mercaptopropionic acid;
the mass fraction of the chain transfer agent in the polymer solution is 0.005% -0.05%.
The initiator is ammonium persulfate solution;
the mass fraction of the initiator in the polymer solution is 0.05% -0.5%.
Preferably or alternatively, the polybasic organic amine is selected from one or a mixture of more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, hydroxyethyl ethylenediamine, hydroxypropyl ethylenediamine and amino ethyl amino propylamine;
the dibasic organic carboxylic acid is selected from one or a mixture of several of succinic acid, glutaric acid, adipic acid and azelaic acid;
the molar ratio of the polybasic organic amine to the dibasic organic carboxylic acid is (1.30-1.01): 1.
Preferably or alternatively, the mass of the polymer a is 5-40% of the mass of the aqueous polyamide polyamine polymer solution.
Preferably or optionally, the following raw materials are used in each step in parts by weight: 0.075-2 parts of epoxy end group monomer containing carbon-carbon double bond, 0.375-5 parts of acrylamide monomer, 0.05-1 part of flexible monomer, 0.05-1 part of cationic monomer, 3.5-8.5 parts of polybasic organic amine, 5-10 parts of dibasic organic carboxylic acid, 0-0.2 part of sodium hydroxide, 0.01-0.2 part of bactericide and 80-90 parts of water.
The invention relates to a preparation method of wrinkling cylinder sticking agent, which has the following beneficial effects compared with the prior art:
1. because the acrylamide monomer, the flexible monomer or the quaternary ammonium salt cationic monomer and the polyamide polyamine polymer are difficult to directly react or polymerize, in the invention, the glycidyl ether allyl alcohol polyoxyethylene ether with vinyl double bond is introduced, and the vinyl can be polymerized with the acrylamide, the flexible monomer and the quaternary ammonium salt cationic monomer by free radicals and then react with the polyamide polyamine polymer, so that the flexible monomer and the quaternary ammonium salt cationic monomer are successfully combined together, and the cohesive force of the product and the hardness of the film reach better levels.
2. According to the invention, glycidyl ether allyl alcohol polyoxyethylene ether is preferably used as an epoxy end group monomer, and because the polyoxyethylene-containing repeating unit has hydrophilicity, the rewettability of the cylinder sticking agent product can be improved, and no humectant such as polyethylene glycol or glycerol is required to be additionally added, so that the product can be applied under the condition of large change of water content of paper sheets.
3. The polymer A of the invention takes the acrylamide monomer as a main body, and provides the binding force of the cylinder adhesive, the paper surface and the drying cylinder surface, which is larger than the binding force of pure PAE resin, thereby meeting the binding force requirement of products in paper machines with different configurations and in the production of different paper products.
4. The flexible monomer with good film forming property and softness is introduced into the polymer A, so that the defects of poor film forming property, hard film coating and the like of a single polyamide polyamine epoxy chloropropane resin adhesive are effectively overcome, and meanwhile, the hand feeling and softness of paper can be improved without adding any additional softener.
5. The invention prefers methacryloxyethyl trimethyl ammonium chloride as cationic monomer, because cationic groups have a strong affinity for a large number of carboxyl groups in the fiber, which can increase the adhesion of the cylinder binder to the paper and drying surfaces.
6. The invention adopts the polymer A with epoxy end groups to carry out crosslinking reaction with the secondary amine groups of the polyamide polyamine polymer, avoids the use of a micromolecular crosslinking agent epichlorohydrin, ensures that the reaction process is more environment-friendly, does not contain organic chlorine byproducts such as DCP, CPD and the like, and ensures that the product can be well used for manufacturing household paper products, and is nontoxic and harmless.
7. The mass of the polymer A solution is designed to be 5-40% of the aqueous polyamide polyamine polymer solution. On the one hand, the epoxy end groups in the polymer A can be fully reacted with the polyamide polyamine polymer, and meanwhile, the flexible monomer can fully play a role to improve the film forming property of the product and reduce the film forming hardness of the product, so that the polymer A is more suitable for being used on a paper machine. On the other hand, the amount of polymer a cannot be too great for cost reasons.
In conclusion, the preparation method has the advantages of relatively low cost, high production efficiency, easiness in reaction control, environment friendliness and the like. The obtained product has high cohesive force, moisture retention, film forming property and film hardness reaching better levels, and can be better combined with fibers, so that the hand feeling of the finished paper is softer.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the invention may be practiced without one or more of these details. In other instances, well-known features have not been described in detail in order to avoid obscuring the invention.
Summary of The Invention
The invention relates to a preparation method of a cylinder sticking agent product which is sprayed onto a yankee dryer to help paper to wrinkle in the manufacturing process of household paper. The defects are overcome by introducing glycidyl ether allyl alcohol polyoxyethylene ether containing epoxy end groups, acrylamide monomers, flexible monomers and quaternary ammonium salt cationic monomer copolymers to react with polyamide polyamine resin, and meanwhile, the film forming property, the hardness and the rewettability of the coating can be adjusted by adding the glycidyl ether allyl alcohol polyoxyethylene ether, the acrylamide monomers, the flexible monomers and the quaternary ammonium salt cationic monomers, so that the requirements of paper making machines of different speeds and types of household papers can be met, and the produced household papers have better handfeel and softness.
Therefore, the wrinkling cylinder adhesive is prepared by reacting a polymer A obtained by free radical polymerization of an epoxy end group monomer containing carbon-carbon double bonds, an acrylamide monomer, a flexible monomer and a quaternary ammonium salt cationic monomer with a polyamide polyamine polymer B, and the specific reaction process is as follows:
1. preparation of Polymer A:
2. preparation of a polyamide polyamine polymer B:
3. preparing wrinkling cylinder sticking agent:
wherein m=8-13, n=180-310, o=12-20, p=7-12, q=9-15, r=8-13, and the m, n, o, p, q, r are positive integers.
The invention is further illustrated below in conjunction with examples, examples of which are intended to illustrate the invention and are not to be construed as limiting the invention. The specific techniques and reaction conditions not specified in the examples may be carried out according to the techniques or conditions described in the literature in this field or the product specifications. Reagents, instruments or equipment not specifically mentioned in the manufacturer are commercially available.
Example 1
30 parts of water, 5 parts of glycidol ether allyl alcohol polyoxyethylene ether 400,6.25 parts of 40% acrylamide aqueous solution (AM-40), 1.875 parts of n-butyl acrylate and 1.875 parts of 80% methacryloxyethyl trimethyl ammonium chloride aqueous solution (DMC-80), regulating the pH of the solution to 3.5-4.5 by 50% sulfuric acid, adding 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite, stirring for dissolving, introducing nitrogen for deoxidizing for half an hour, then slowly heating to 70 ℃, slowly dropwise adding 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution (AM-40) for 2 hours, preserving the temperature at 75-85 ℃ for 4 hours after the dropwise adding, stopping heating, then adding a proper amount of water to regulate the solid content to 15wt%, and cooling to room temperature to obtain a polymer A solution.
26 parts of diethylenetriamine is added into a reaction bottle, then 32 parts of adipic acid is slowly added under the stirring state, the temperature is raised to 150 ℃ after the mixture is stirred uniformly, the generated water is continuously distilled out, after the reaction is carried out for 1 hour, the temperature is raised to 165 ℃, the reaction is continued for 4 hours, then 22 parts of warm water is slowly added to terminate the reaction, finally a proper amount of dilution water is added, and the polyamide polyamine polymer B with 50% of solid content can be obtained after the mixture is stirred uniformly.
27 parts of polyamide polyamine polymer is added into a reaction flask, 18 parts of water is added to regulate the solid content, then 9 parts of polymer A solution (solid content is 15%) is added dropwise, the temperature is raised to 60 ℃ for reaction for 2-2.5 hours, the viscosity is measured by sampling every 15 minutes after the reaction is carried out for 1.5 hours at 60 ℃, and the reaction is stopped when the solution viscosity reaches 250-400mPa.s, so that a reactant is obtained. Cooling the materials to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
Example 2
30 parts of water, 5 parts of glycidol ether allyl alcohol polyoxyethylene ether 600,6.25 parts of 40% acrylamide aqueous solution (AM-40), 1.875 parts of isobutyl acrylate and 1.875 parts of 80% methacryloxyethyl trimethyl ammonium chloride aqueous solution (DMC-80), regulating the pH of the solution to 3.5-4.5 by 50% sulfuric acid, adding 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite, stirring for dissolving, introducing nitrogen for deoxidizing for half an hour, then slowly heating to 70 ℃, slowly dropwise adding 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution (AM-40) for 2 hours, preserving the heat at 75-85 ℃ for 4 hours after the dropwise adding, stopping heating, then adding a proper amount of water to regulate the solid content to 15wt%, and cooling to room temperature to obtain a polymer A solution.
26.5 parts of diethylenetriamine is added into a reaction bottle, 31.5 parts of adipic acid is slowly added under the stirring state, the temperature is raised to 150 ℃ after the stirring is uniform, the generated water is continuously distilled out, after the reaction is carried out for 1 hour, the temperature is raised to 165 ℃, the reaction is continued for 4 hours, then 22 parts of warm water is slowly added to terminate the reaction, finally a proper amount of dilution water is added, and the polyamide polyamine polymer B with 50% of solid content can be obtained after the stirring is uniform.
27 parts of polyamide polyamine polymer is added into a reaction flask, 18 parts of water is added to regulate the solid content, then 9.2 parts of polymer A solution (the solid content is 15%) is added dropwise, the temperature is raised to 60 ℃ for reaction for 2 to 2.5 hours, the viscosity is measured by sampling every 15 minutes after the reaction is carried out for 1.5 hours at 60 ℃, and the reaction is stopped when the solution viscosity reaches 250 to 400mPa.s, so that a reactant is obtained. Cooling the materials to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
Example 3
30 parts of water, 5 parts of Glycidyl Methacrylate (GMA), 6.25 parts of 40% acrylamide aqueous solution (AM-40), 1.875 parts of isobutyl acrylate and 3.0 parts of 50% methacrylamidopropyl trimethyl ammonium chloride (MAPTAC) are added into a reaction bottle, the pH value of the solution is regulated to 3.5-4.5 by 50% sulfuric acid, 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite are added, stirring and dissolving are carried out, nitrogen is introduced for half an hour, then the temperature is slowly increased to 70 ℃, 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution (AM-40) are slowly added dropwise, the dropwise addition time is 2 hours, the temperature is kept at 75-85 ℃ for 4 hours after the dropwise addition, heating is stopped, then a proper amount of water is added to regulate the solid content to 15wt%, and the solution is cooled to room temperature, thus obtaining polymer A solution.
21 parts of triethylene tetramine is added into a reaction bottle, then 21 parts of adipic acid is slowly added under the stirring state, the temperature is raised to 150 ℃ after the mixture is stirred uniformly, the generated water is continuously distilled out, after the reaction is carried out for 1 hour, the temperature is raised to 175 ℃, the reaction is continued for 4 hours, then 20 parts of warm water is slowly added to terminate the reaction, finally a proper amount of dilution water is added, and the polyamide polyamine polymer B with 50% of solid content can be obtained after the mixture is stirred uniformly.
27.5 parts of polyamide polyamine polymer is added into a reaction flask, 18.2 parts of water is added to regulate the solid content, then 9.1 parts of polymer A solution (the solid content is 15%) is dropwise added, the temperature is raised to 60 ℃ for reaction for 2 to 2.5 hours, the viscosity is measured by sampling every 15 minutes after the reaction is carried out for 1.5 hours at 60 ℃, and the reaction is stopped when the solution viscosity reaches 250 to 400mPa.s, so that a reactant is obtained. Cooling the materials to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
Example 4
30 parts of water, 5 parts of Allyl Glycidyl Ether (AGE), 6.25 parts of 40% acrylamide aqueous solution (AM-40), 1.875 parts of isobutyl acrylate and 2.5 parts of 60% dimethyl diallyl ammonium chloride (DMDAAC) are added into a reaction bottle, the pH value of the solution is regulated to 3.5-4.5 by 50% sulfuric acid, 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite are added, stirring and dissolving are carried out, nitrogen is introduced for deoxidization for half an hour, then the temperature is slowly increased to 70 ℃, 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution (AM-40) are slowly added dropwise, the dropwise addition time is 2 hours, the temperature is kept at 75-85 ℃ for 4 hours after the dropwise addition, heating is stopped, then a proper amount of water is added to regulate the solid content to 15wt%, and the solution is cooled to room temperature, thus obtaining polymer A solution.
21 parts of triethylene tetramine is added into a reaction bottle, then 21 parts of adipic acid is slowly added under the stirring state, the temperature is raised to 150 ℃ after the mixture is stirred uniformly, the generated water is continuously distilled out, after the reaction is carried out for 1 hour, the temperature is raised to 175 ℃, the reaction is continued for 4 hours, then 20 parts of warm water is slowly added to terminate the reaction, finally a proper amount of dilution water is added, and the polyamide polyamine polymer B with 50% of solid content can be obtained after the mixture is stirred uniformly.
27.5 parts of polyamide polyamine polymer is added into a reaction flask, 18.2 parts of water is added to regulate the solid content, then 9.2 parts of polymer A solution (the solid content is 15%) is dropwise added, the temperature is raised to 60 ℃ for reaction for 2 to 2.5 hours, the viscosity is measured by sampling every 15 minutes after the reaction is carried out for 1.5 hours at 60 ℃, and the reaction is stopped when the solution viscosity reaches 250 to 400mPa.s, so that a reactant is obtained. Cooling the materials to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
Comparative example 1
26.5 parts of diethylenetriamine is added into a reaction bottle, 31.5 parts of adipic acid is slowly added under the stirring state, the temperature is raised to 150 ℃ after the stirring is uniform, the generated water is continuously distilled out, after the reaction is carried out for 1 hour, the temperature is raised to 165 ℃, the reaction is continued for 4 hours, then 22 parts of warm water is slowly added to terminate the reaction, finally a proper amount of dilution water is added, and the polyamide polyamine polymer with 50% of solid content can be obtained after the stirring is uniform.
26.6 parts of polyamide polyamine polymer is added into a reaction flask, 17 parts of water is added to regulate the solid content, then 1.3 parts of epichlorohydrin is added dropwise, the temperature is raised to 60 ℃ for reaction for 2 to 2.5 hours, the viscosity is measured by sampling every 15 minutes after the reaction is carried out for 1.5 hours at 60 ℃, and the reaction is stopped by adding water when the solution viscosity reaches 250 to 400mPa.s, thus obtaining the reactant. Cooling the materials to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
Comparative example 2
21 parts of triethylene tetramine is added into a reaction bottle, then 21 parts of adipic acid is slowly added under the stirring state, the temperature is raised to 150 ℃ after the mixture is stirred uniformly, the generated water is continuously distilled off, after the reaction is carried out for 1 hour, the temperature is raised to 175 ℃, the reaction is continued for 4 hours, then 20 parts of warm water is slowly added to terminate the reaction, finally a proper amount of dilution water is added, and the polyamide polyamine polymer with 50% of solid content can be obtained after the mixture is stirred uniformly.
26.6 parts of polyamide polyamine polymer is added into a reaction flask, 17 parts of water is added to regulate the solid content, then 1.4 parts of epichlorohydrin is added dropwise, the temperature is raised to 65 ℃ for 2 to 2.5 hours, the reaction is carried out for 1.5 hours at 65 ℃ and then the viscosity is measured by sampling every 15 minutes, and when the solution viscosity reaches 300 to 450mPa.s, the reaction is stopped by adding water, thus obtaining the reactant. Cooling the materials to below 35 ℃, adding 0.05 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
The cylinder sticking agent samples and the comparative samples (commercially available product 1 and commercially available product 2, both of which were polyamide-epichlorohydrin resin cylinder sticking agents) prepared in examples 1 to 4 and comparative examples 1 to 2 were respectively subjected to tests of viscosity, pH, solid content, adhesion, film hardness and rewettability, wherein the solid content was tested by an oven method, the pH was tested at 25℃by a conventional pH meter, the viscosity was tested by a conventional Brookfiled viscometer (25℃in mPas), and the adhesion was tested by the method disclosed in the preparation of a polyamide-epichlorohydrin resin cylinder sticking agent of patent CN101235610A (Kg in Kg) by the following method: spraying the cylinder sticking agent onto a stainless steel platform heated to 110 ℃, and performing coating scratch experiments by using pencils with different hardness after the cylinder sticking agent is solidified into a film. Test methods for rewettability refer to CN103415550B polyamine polyamidoamine epihalohydrin compositions and methods disclosed in methods of making and using the same. The specific test results are shown in the following table:
discussion of the invention
Based on the above test results, we can find that: examples 1 to 4, compared with the comparative example, commercially available products, by introducing glycidyl ether-based allyl alcohol polyoxyethylene ether having a vinyl double bond, it is possible to improve the rewettability of the cylinder adhesive product by free radical polymerization of the vinyl group with acrylamide, a flexible monomer and a quaternary ammonium salt cationic monomer, and then reacting with a polyamide polyamine polymer to thereby successfully bond the two together, since the glycidyl ether-based allyl alcohol polyoxyethylene ether is used as an epoxy-terminated monomer, containing a large amount of polyoxyethylene repeating units having hydrophilicity; the flexible monomer with good film forming property and softness is introduced, so that the defects of poor film forming property, hard film coating and the like of a single polyamide polyamine epoxy chloropropane resin adhesive are effectively overcome, and meanwhile, the hand feeling and softness of paper can be improved without adding any additional softener; the methyl methacrylate oxyethyl trimethyl ammonium chloride is selected as a cationic monomer, and the cationic group has stronger affinity for a large number of carboxyl groups in the fiber, so that the binding force between the cylinder adhesive and paper and drying cylinder surfaces can be increased.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
Claims (4)
1. A method for preparing a wrinkling cylinder adhesive, which is characterized by comprising the following steps:
adding 30 parts of water, 5 parts of glycidyl ether allyl alcohol polyoxyethylene ether 400,6.25 parts of 40% acrylamide aqueous solution, 1.875 parts of n-butyl acrylate and 1.875 parts of 80% methacryloyloxyethyl trimethyl ammonium chloride aqueous solution into a reaction bottle, regulating the pH of the solution to 3.5-4.5 by using 50% sulfuric acid, adding 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite, stirring for dissolving, introducing nitrogen to remove oxygen for half an hour, then slowly heating to 70 ℃, slowly dropwise adding 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution for 2 hours, preserving heat for 4 hours at 75-85 ℃ after the dropwise adding is finished, stopping heating, then adding a proper amount of water to regulate the solid content to 15wt%, and cooling to room temperature to obtain a polymer A solution;
adding 26 parts of diethylenetriamine into a reaction bottle, slowly adding 32 parts of adipic acid under a stirring state, heating to 150 ℃ after stirring uniformly, continuously steaming out generated water, heating to 165 ℃ after reacting for 1 hour, continuing to react for 4 hours, slowly adding 22 parts of warm water to terminate the reaction, finally adding a proper amount of dilution water, and stirring uniformly to obtain a polyamide polyamine polymer B solution with the solid content of 50%;
adding 27 parts of polyamide polyamine polymer B solution into a reaction flask, adding 18 parts of water to regulate the solid content, then dropwise adding 9 parts of polymer A solution, heating to 60 ℃ to react for 2-2.5 hours, sampling every 15 minutes to measure the viscosity after reacting for 1.5 hours at 60 ℃, and adding water to terminate the reaction when the solution viscosity reaches 250-400mPa.s to obtain a reactant;
cooling the reactants to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
2. A method for preparing a wrinkling cylinder adhesive, which is characterized by comprising the following steps:
adding 30 parts of water, 5 parts of glycidyl ether allyl alcohol polyoxyethylene ether 600,6.25 parts of 40% acrylamide aqueous solution, 1.875 parts of isobutyl acrylate and 1.875 parts of 80% methacryloyloxyethyl trimethyl ammonium chloride aqueous solution into a reaction bottle, regulating the pH of the solution to 3.5-4.5 by using 50% sulfuric acid, adding 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite, stirring for dissolving, introducing nitrogen for deoxidizing for half an hour, then slowly heating to 70 ℃, slowly dropwise adding 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution for 2 hours, preserving heat for 4 hours at 75-85 ℃ after the dropwise adding, stopping heating, then adding a proper amount of water to regulate the solid content to 15wt%, and cooling to room temperature to obtain a polymer A solution;
adding 26.5 parts of diethylenetriamine into a reaction bottle, slowly adding 31.5 parts of adipic acid under a stirring state, heating to 150 ℃ after stirring uniformly, continuously steaming out generated water, heating to 165 ℃ after reacting for 1 hour, continuing to react for 4 hours, slowly adding 22 parts of warm water to terminate the reaction, finally adding a proper amount of dilution water, and stirring uniformly to obtain a polyamide polyamine polymer B solution with 50% of solid content;
adding 27 parts of polyamide polyamine polymer B solution into a reaction flask, adding 18 parts of water to regulate the solid content, then dropwise adding 9.2 parts of polymer A solution, heating to 60 ℃ to react for 2-2.5 hours, sampling every 15 minutes after reacting for 1.5 hours at 60 ℃, measuring the viscosity, and adding water to terminate the reaction when the solution viscosity reaches 250-400mPa.s to obtain a reactant;
cooling the reactants to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
3. A method for preparing a wrinkling cylinder adhesive, which is characterized by comprising the following steps:
adding 30 parts of water, 5 parts of glycidyl methacrylate, 6.25 parts of 40% acrylamide aqueous solution, 1.875 parts of isobutyl acrylate and 3.0 parts of 50% methacrylamidopropyl trimethyl ammonium chloride into a reaction bottle, regulating the pH of the solution to 3.5-4.5 by using 50% sulfuric acid, adding 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite, stirring for dissolving, introducing nitrogen and deoxidizing for half an hour, then slowly heating to 70 ℃, slowly dropwise adding 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution, keeping the temperature at 75-85 ℃ for 4 hours after the dropwise adding is finished, stopping heating, then adding a proper amount of water to regulate the solid content to 15wt%, and cooling to room temperature to obtain a polymer A solution;
adding 21 parts of triethylene tetramine into a reaction bottle, slowly adding 21 parts of adipic acid under a stirring state, heating to 150 ℃ after stirring uniformly, continuously steaming out generated water, heating to 175 ℃ after reacting for 1 hour, continuing to react for 4 hours, slowly adding 20 parts of warm water to terminate the reaction, finally adding a proper amount of dilution water, and stirring uniformly to obtain a polyamide polyamine polymer B solution with the solid content of 50%;
adding 27.5 parts of polyamide polyamine polymer B solution into a reaction flask, adding 18.2 parts of water to regulate the solid content, then dropwise adding 9.1 parts of polymer A solution, heating to 60 ℃ for reaction for 2-2.5 hours, sampling and measuring the viscosity every 15 minutes after reacting for 1.5 hours at 60 ℃, and adding water to terminate the reaction when the solution viscosity reaches 250-400mPa.s to obtain a reactant;
cooling the reactants to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
4. A method for preparing a wrinkling cylinder adhesive, which is characterized by comprising the following steps:
adding 30 parts of water, 5 parts of allyl glycidyl ether, 6.25 parts of 40% acrylamide aqueous solution, 1.875 parts of isobutyl acrylate and 2.5 parts of 60% dimethyl diallyl ammonium chloride into a reaction bottle, regulating the pH of the solution to 3.5-4.5 by using 50% sulfuric acid, adding 0.01 part of EDTA-Na2 and 0.02 part of sodium hypophosphite, stirring for dissolving, introducing nitrogen to remove oxygen for half an hour, slowly heating to 70 ℃, slowly dropwise adding 0.6 part of 3% ammonium persulfate solution and 10 parts of 40% acrylamide aqueous solution for 2 hours, preserving heat at 75-85 ℃ for 4 hours after the dropwise addition is finished, stopping heating, then adding a proper amount of water to regulate the solid content to 15wt%, and cooling to room temperature to obtain a polymer A solution;
adding 21 parts of triethylene tetramine into a reaction bottle, slowly adding 21 parts of adipic acid under a stirring state, heating to 150 ℃ after stirring uniformly, continuously steaming out generated water, heating to 175 ℃ after reacting for 1 hour, continuing to react for 4 hours, slowly adding 20 parts of warm water to terminate the reaction, finally adding a proper amount of dilution water, and stirring uniformly to obtain a polyamide polyamine polymer B solution with the solid content of 50%;
adding 27.5 parts of polyamide polyamine polymer B solution into a reaction flask, adding 18.2 parts of water to regulate the solid content, then dropwise adding 9.2 parts of polymer A solution, heating to 60 ℃ to react for 2-2.5 hours, reacting at 60 ℃ for 1.5 hours, sampling and measuring the viscosity every 15 minutes, and adding water to stop the reaction when the solution viscosity reaches 250-400mPa.s to obtain a reactant;
cooling the reactants to below 35 ℃, adding 0.02 part of 10% liquid alkali to adjust the pH, then adding 0.1 part of bactericide BIT-20, and finally adding water to adjust the solid content to 15%, thus obtaining the cylinder sticking agent product.
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