CN106750475A - 一种具有高抗返渗性能的高吸水性树脂的制备方法 - Google Patents
一种具有高抗返渗性能的高吸水性树脂的制备方法 Download PDFInfo
- Publication number
- CN106750475A CN106750475A CN201710106337.4A CN201710106337A CN106750475A CN 106750475 A CN106750475 A CN 106750475A CN 201710106337 A CN201710106337 A CN 201710106337A CN 106750475 A CN106750475 A CN 106750475A
- Authority
- CN
- China
- Prior art keywords
- absorbent resin
- super absorbent
- returning
- preparation
- height
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002250 absorbent Substances 0.000 title claims abstract description 40
- 230000002745 absorbent Effects 0.000 title claims abstract description 40
- 239000011347 resin Substances 0.000 title claims abstract description 39
- 229920005989 resin Polymers 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000008187 granular material Substances 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000000017 hydrogel Substances 0.000 claims abstract description 22
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003292 glue Substances 0.000 claims abstract description 20
- 238000005469 granulation Methods 0.000 claims abstract description 19
- 230000003179 granulation Effects 0.000 claims abstract description 19
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 17
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 10
- 239000004088 foaming agent Substances 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims abstract description 10
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 43
- 239000000693 micelle Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 12
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 12
- 238000006386 neutralization reaction Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 230000000977 initiatory effect Effects 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- XRRONFCBYFZWTM-UHFFFAOYSA-N octadecanoic acid;sodium Chemical compound [Na].CCCCCCCCCCCCCCCCCC(O)=O XRRONFCBYFZWTM-UHFFFAOYSA-N 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- -1 azo diisobutyl ether hydrochloric acid Salt Chemical compound 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229960003511 macrogol Drugs 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical class OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 5
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 5
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- KDNYCTPSPZHJQF-UHFFFAOYSA-N 3-phenylbutan-2-ol Chemical compound CC(O)C(C)C1=CC=CC=C1 KDNYCTPSPZHJQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004258 Ethoxyquin Substances 0.000 claims description 3
- 229920002538 Polyethylene Glycol 20000 Polymers 0.000 claims description 3
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 3
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 3
- DECIPOUIJURFOJ-UHFFFAOYSA-N ethoxyquin Chemical compound N1C(C)(C)C=C(C)C2=CC(OCC)=CC=C21 DECIPOUIJURFOJ-UHFFFAOYSA-N 0.000 claims description 3
- 229940093500 ethoxyquin Drugs 0.000 claims description 3
- 235000019285 ethoxyquin Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- UEMGWPRHOOEKTA-UHFFFAOYSA-N 1,3-difluorobenzene Chemical compound FC1=CC=CC(F)=C1 UEMGWPRHOOEKTA-UHFFFAOYSA-N 0.000 claims description 2
- IQXJCCZJOIKIAD-UHFFFAOYSA-N 1-(2-methoxyethoxy)hexadecane Chemical compound CCCCCCCCCCCCCCCCOCCOC IQXJCCZJOIKIAD-UHFFFAOYSA-N 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical class C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 claims description 2
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims description 2
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical compound [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 claims description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 229950009789 cetomacrogol 1000 Drugs 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 claims description 2
- 229940093430 polyethylene glycol 1500 Drugs 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims 1
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Natural products C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 claims 1
- 125000005147 toluenesulfonyl group Chemical group C=1(C(=CC=CC1)S(=O)(=O)*)C 0.000 claims 1
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000003999 initiator Substances 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 17
- 239000000178 monomer Substances 0.000 description 7
- 230000007935 neutral effect Effects 0.000 description 7
- 150000001253 acrylic acids Chemical class 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 5
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 description 2
- UKTDQTGMXUHPIF-UHFFFAOYSA-N [Na].S(O)(O)=O Chemical compound [Na].S(O)(O)=O UKTDQTGMXUHPIF-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229940085675 polyethylene glycol 800 Drugs 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- DTNNSSFOAYQGOZ-UHFFFAOYSA-N 1-butoxybutane;hydrochloride Chemical compound Cl.CCCCOCCCC DTNNSSFOAYQGOZ-UHFFFAOYSA-N 0.000 description 1
- MEJAPGGFIJZHEJ-UHFFFAOYSA-N 5-acetamido-1,3,4-thiadiazole-2-sulfonyl chloride Chemical compound CC(=O)NC1=NN=C(S(Cl)(=O)=O)S1 MEJAPGGFIJZHEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- CKVXWQNCJMOEFA-UHFFFAOYSA-N C(C=C)(=O)OC(C(OC(C=C)=O)(COC(C=C)=O)OCC)(OCC)OCC Chemical compound C(C=C)(=O)OC(C(OC(C=C)=O)(COC(C=C)=O)OCC)(OCC)OCC CKVXWQNCJMOEFA-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 206010021639 Incontinence Diseases 0.000 description 1
- DJOWTWWHMWQATC-KYHIUUMWSA-N Karpoxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1(O)C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C DJOWTWWHMWQATC-KYHIUUMWSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007046 ethoxylation reaction Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 238000005213 imbibition Methods 0.000 description 1
- SZNYYWIUQFZLLT-UHFFFAOYSA-N isopropylmethyl ether Natural products CC(C)COCC(C)C SZNYYWIUQFZLLT-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229940117969 neopentyl glycol Drugs 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
- C08J9/105—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof containing sulfur
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
- A61F2013/530481—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium having superabsorbent materials, i.e. highly absorbent polymer gel materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/022—Hydrogel, i.e. a gel containing an aqueous composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Biomedical Technology (AREA)
- Epidemiology (AREA)
- Heart & Thoracic Surgery (AREA)
- Vascular Medicine (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Laminated Bodies (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明是一种具有高抗返渗性能的高吸水性树脂的制备方法，其方法如下：首先使用碱将丙烯酸水溶液进行中和，加入复合引发剂、交联剂及发泡剂后在UV光照射下进行聚合反应；然后对聚合后的水凝胶进行切碎造粒，切碎过程中均匀加入切胶助剂，后经干燥、粉碎后得高吸水性树脂初级颗粒；最后在初级颗粒表面喷涂表面交联液，在高温下反应后得高吸水性树脂最终产品。本方法制得的高吸水性树脂具有吸收倍率高、吸收速度快、保水性能好、抗返渗性能优异等特点。
Description
技术领域
本发明涉及一种聚丙烯酸盐类高吸水性树脂的制备方法，特别是一种具有高抗返渗性能的高吸水性树脂的制备方法。
背景技术
高吸水性树脂是继棉花、海绵等传统吸水性材料之后的新一代吸水性功能高分子材料。相对于传统吸水材料，高吸水性树脂的吸收量能够达到自身重量成百上千倍，并且在吸水后具有较好的保水性能，加压条件下也能实现较高的吸收量，这均得益于其含有大量亲水性基团的三维网状弹性结构特性。近年来高吸水性树脂得到了高速发展，国内高吸水性树脂生产装置的数量及产能均在逐步扩大，但是现有产品通常存在着吸水溶胀后在一定压力下返渗量较大的问题，严重影响了产品的应用体验。
发明内容
本发明所要解决的技术问题是针对现有技术存在的问题，提供一种具有高抗返渗性能的高吸水性树脂的制备方法，该方法制得的高吸水性树脂吸收倍率高，吸液速度快，保水性能好，抗返渗性能优异。
本发明所要解决的技术问题是通过以下的技术方案来实现的，本发明是一种具有高抗返渗性能的高吸水性树脂的制备方法，其特点是：其步骤如下：
（1）将丙烯酸加水稀释后，在冰水浴中加入氢氧化钠中和制得中和液，中和液的中和度为0%-80%，其中丙烯酸质量占中和液总质量的20%-35%；
（2）在中和液中加入复合光引发剂、交联剂和发泡剂搅拌均匀后，在UV光照射下进行聚合反应，控制聚合起始温度为0-60℃，得到水凝胶；所述复合光引发剂质量为中和液中丙烯酸总量的0.001%-0.3%；所述交联剂质量为中和液中丙烯酸总量的0.01%-0.6%；所述发泡剂质量为中和液中丙烯酸总量的0.01%-3%；
（3）将水凝胶加入切胶造粒机中造粒，造粒过程中均匀加入切胶助剂，制得胶粒，胶粒干燥、粉碎后得初级颗粒；所述切胶助剂的质量为水凝胶质量的2%-15%；
（4）将步骤（3）得到的初级颗粒表面喷涂表面交联液，经热处理后制得最终产品；所述的表面交联液由丙二醇、乙二醇二缩水甘油醚和硫酸盐混合组成，其中丙二醇质量为初级颗粒总质量的0.01-2%；乙二醇二缩水甘油醚质量为初级颗粒总质量的0.005%-0.5%；硫酸盐质量为初级颗粒质量的0.1-4.0%。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（2）中，所述的UV光的波长为150-350nm，光照时间为1-30min，反应结束后水凝胶的最高温度为70-100℃。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（2）中，所述复合光引发剂为1-羟基环已基苯基甲酮、2,2-二甲氧基-2-苯基苯乙酮、苯基双(2,4,6-三甲基苯甲酰基)氧化膦、2-苯基苄-2-二甲基胺-1-（4-吗啉苄苯基）丁酮、2-羟基-甲基苯基丙烷-1-酮、双(1-(2,4-二氟苯基)-3-吡咯基)二茂钛、偶氮二异丁醚盐酸盐、二苯基-(2,4,6-三甲基苯甲酰)氧磷、2-甲基-1-(4-甲硫基苯基 )-2-吗啉基-1-丙酮、过硫酸铵、过硫酸钠中的至少一种。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（2）中，所述交联剂为聚乙二醇200、聚乙二醇300、聚乙二醇400、聚乙二醇600、聚乙二醇800、聚乙二醇1000、聚乙二醇1500、聚乙二醇2000、聚乙二醇4000、聚乙二醇6000、聚乙二醇10000、聚乙二醇20000、季戊四醇三丙烯酸酯、季戊四醇三烯丙基醚、二季戊四醇五丙烯酸酯、乙氧化三羟甲基丙烷三丙烯酸酯、1，4-丁二醇二丙烯酸酯;1，6-己二醇二丙烯酸酯、新戊二醇二丙烯酸酯、丙氧基化新戊二醇二丙烯酸酯、乙氧基化新戊二醇二丙烯酸酯、三乙氧基化甘油三丙烯酸酯、乙二醇二缩水甘油醚中的至少一种。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（2）中，所述发泡剂为碳酸氢钠、碳酸氢钾、碳酸氢铵、碳酸钠、碳酸钾、甲苯磺酰肼、4,4-氧代双苯磺酰肼、气相二氧化硅中的至少一种。其中碳酸氢钠、碳酸钠、氢氧化钠、氢氧化钾主要用于调整凝胶中丙烯酸单体的总中和度，从而使凝胶PH值达到偏中性。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（3）中，所述切胶助剂为硬质酸钠、碳酸氢钠、碳酸钠、氢氧化钠、氢氧化钾、蔗糖酯、亚硫酸钠、焦亚硫酸钠中的两种或两种以上。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（3）中胶粒的干燥温度为70-220℃。
本发明所述的具有高抗返渗性能的高吸水性树脂的制备方法，其进一步优选的技术方案是：步骤（4）中热处理温度为70-220℃。
本发明采用了复合引发方式，在缩短聚合反应时间的同时，提高了凝胶分子量的均匀性；通过聚合过程中引入发泡剂增加了凝胶内的孔洞，提高了颗粒内表面积；通过在切胶时加入切胶助剂提高了颗粒表面的粗糙程度；从而在提高高吸水性树脂性能指标的同时显著提高了其吸液速度及抗返渗性能。
与现有技术相比，本发明具有吸收倍率高、吸液速度快，保水性能好、抗返渗性能优异等特点，适用于超干爽婴儿纸尿裤、卫生巾以及成人失禁用品等领域。
具体实施方式
以下进一步描述本发明的具体技术方案，以便于本领域的技术人员进一步地理解本发明，而不构成对其权利的限制。
实施例1，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将丙烯酸加水稀释后，在冰水浴中加入氢氧化钠中和制得中和液，中和液的中和度为0%-80%，其中丙烯酸质量占中和液总质量的20%-35%；
（2）在中和液中加入复合光引发剂、交联剂和发泡剂搅拌均匀后，在UV光照射下进行聚合反应，控制聚合起始温度为0-60℃，得到水凝胶；所述复合光引发剂质量为中和液中丙烯酸总量的0.001%-0.3%；所述交联剂质量为中和液中丙烯酸总量的0.01%-0.6%；所述发泡剂质量为中和液中丙烯酸总量的0.01%-3%；
（3）将水凝胶加入切胶造粒机中造粒，造粒过程中均匀加入切胶助剂，制得胶粒，胶粒干燥、粉碎后得初级颗粒；所述切胶助剂的质量为水凝胶质量的2%-15%；
（4）将步骤（3）得到的初级颗粒表面喷涂表面交联液，经热处理后制得最终产品；所述的表面交联液由丙二醇、乙二醇二缩水甘油醚和硫酸盐混合组成，其中丙二醇质量为初级颗粒总质量的0.01-2%；乙二醇二缩水甘油醚质量为初级颗粒总质量的0.005%-0.5%；硫酸盐质量为初级颗粒质量的0.1-4.0%。
实施例2，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将200g高纯丙烯酸加466g水稀释后，在冰水浴中加入50%氢氧化钠150g中和制得中和液；
（2）在中和液中加入2,2-二甲氧基-2-苯基苯乙酮0.05g、过硫酸钠0.8g、聚乙二醇600为0.4g及碳酸氢钠2g搅拌均匀后，控制聚合起始温度为7℃，在UV光照射下引发聚合反应，UV光波长为150-350nm，光照30min后得到水凝胶；
（3）将水凝胶加入切胶造粒机中造粒，制得胶粒，造粒过程中均匀加入碳酸钠10g调整凝胶中丙烯酸单体的中和度，使凝胶PH值达到偏中性，再均匀加入硬质酸钠0.10g、亚硫酸钠5.0g，胶粒在190℃温度下干燥60min，后粉碎得初级颗粒；
（4）将步骤（3）得到的初级颗粒表面喷涂由丙二醇1g、乙二醇二缩水甘油醚0.05g、硫酸盐2.6g和去离子水6g混合后的表面交联液，经160℃热处理后制得最终产品。
实施例3，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将190g高纯丙烯酸加515g水稀释后，在冰水浴中加入50%氢氧化钠84g中和制得中和液;
（2）在中和液中加入2,2-二甲氧基-2-苯基苯乙酮0.04g、过硫酸钠0.75g、聚乙二醇400为0.36g及碳酸氢钠2.5g搅拌均匀后，控制聚合起始温度为6℃，在UV光照射下引发聚合反应，光照30min后得到水凝胶；
（3）将水凝胶加入切胶造粒机中造粒，制得胶粒，造粒过程中均匀加入50%氢氧化钠63g调整凝胶中丙烯酸单体的中和度，使凝胶PH值达到偏中性，再均匀加入硬质酸钠0.10g、焦亚硫酸钠5.0g，胶粒在200℃温度下干燥60min，粉碎后得初级颗粒；
（4）将步骤（3）得到的初级颗粒表面喷涂由丙二醇0.9g、乙二醇二缩水甘油醚0.06g、硫酸盐2.8g和去离子水5.8g混合后的表面交联液，经160℃热处理后制得最终产品。
实施例4，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将220g高纯丙烯酸加510g水稀释后，在冰水浴中加入50%氢氧化钠49g中和制得中和液;
（2）在中和液中加入2,2-二甲氧基-2-苯基苯乙酮0.05g、过硫酸钠0.9g、聚乙二醇600为0.27g、季戊四醇三丙烯酸酯0.27g及碳酸氢钠2.4g搅拌均匀后，控制聚合起始温度为8℃，在UV光照射下引发聚合反应，光照30min后得到水凝胶；
（3）将水凝胶加入切胶造粒机中造粒，制得胶粒，造粒过程中均匀加入50%氢氧化钠141g调整凝胶中丙烯酸单体的中和度，使凝胶PH值达到偏中性，再均匀加入硬质酸钠0.10g、焦亚硫酸钠4.6g，胶粒在180℃温度下干燥60min，粉碎后得初级颗粒；
（4）将步骤（3）得到的初级颗粒表面喷涂由丙二醇1.3g、乙二醇二缩水甘油醚0.07g、硫酸盐2.8g、硫酸钠0.2g和去离子水8g混合后的表面交联液，经160℃热处理后制得最终产品。
实施例5，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将210g高纯丙烯酸加604g水稀释后，在冰水浴中加入50%氢氧化钠116g中和制得中和液;
（2）在中和液中加入2,2-二甲氧基-2-苯基苯乙酮0.05g、过硫酸铵0.6g、偶氮二异丁醚盐酸盐0.3g、乙氧化三羟甲基丙烷三丙烯酸酯0.4g及碳酸氢钠2.2g搅拌均匀后，控制聚合起始温度为9℃，在UV光照射下引发聚合反应，光照30min后得到水凝胶；
（3）将水凝胶加入切胶造粒机中造粒，制得胶粒，造粒过程中均匀加入碳酸钠42g调整凝胶中丙烯酸单体的中和度，使凝胶PH值达到偏中性，再均匀加入硬质酸钠0.12g、亚硫酸钠5g，胶粒在190℃温度下干燥50min，粉碎后得初级颗粒；
（4）将步骤（3）得到的初级颗粒表面喷涂由丙二醇1.2g、乙二醇二缩水甘油醚0.06g、硫酸铝2.9g和去离子水7.5g混合后的表面交联液，经150℃热处理后制得最终产品。
实施例6，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将200g高纯丙烯酸加483g水稀释后，在冰水浴中加入50%氢氧化钠33g中和制得中和液;
（2）在中和液中加入2-羟基-甲基苯基丙烷-1-酮0.05g、过硫酸钠0.8g、聚乙二醇800为0.5g及4,4-氧代双苯磺酰肼3g搅拌均匀后，控制聚合起始温度为9℃，在UV光照射下引发聚合反应，光照30min后得到水凝胶；
（3）将水凝胶加入切胶造粒机中造粒，制得胶粒，造粒过程中均匀加入50%氢氧化钠144g调整凝胶中丙烯酸单体的中和度，使凝胶PH值达到偏中性，再均匀加入蔗糖酯0.12g、焦亚硫酸钠5g，胶粒在160℃温度下干燥60min，粉碎后得初级颗粒；
（4）将步骤（3）得到的初级颗粒表面喷涂由丙二醇1.1g、乙二醇二缩水甘油醚0.06g、硫酸铝2.4g、硫酸钠0.3g和去离子水7g混合后的表面交联液，经150℃热处理后制得最终产品。
实施例7，一种具有高抗返渗性能的高吸水性树脂的制备方法，其步骤如下：
（1）将200g高纯丙烯酸加428g水稀释，配成丙烯酸稀释液；
（2）在稀释液中加入2,2-二甲氧基-2-苯基苯乙酮0.05g、过硫酸铵0.8g、季戊四醇三烯丙基醚0.4g及碳酸氢钠2.2g搅拌均匀后，控制聚合起始温度为5℃，在UV光照射下引发聚合反应，光照30min后得到水凝胶；
（3）将水凝胶加入切胶造粒机中造粒，制得胶粒，造粒过程中均匀加入50%氢氧化钠166g调整凝胶中丙烯酸单体的中和度，使凝胶PH值达到偏中性，再均匀加入硬质酸钠0.12g、焦亚硫酸钠5g，胶粒在160℃温度下干燥60min，粉碎后得初级颗粒；
（4）将步骤（3）得到的初级颗粒表面喷涂由丙二醇1.1g、乙二醇二缩水甘油醚0.06g、硫酸铝2.7g和去离子水6g混合后的表面交联液，经150℃热处理后制得最终产品。
将实施例2、3、4、5、6和7制得的高吸水性树脂进行检测，测试的数据如表1：
表1：
由此可知本方法制得的高吸水性树脂具有吸收倍率高、吸收速度快、保水性能好、抗返渗性能优异等特点。
Claims (8)
1.一种具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于，其步骤如下：
（1）将丙烯酸加水稀释后，在冰水浴中加入氢氧化钠中和制得中和液，中和液的中和度为0%-80%，其中丙烯酸质量占中和液总质量的20%-35%；
（2）在中和液中加入复合光引发剂、交联剂和发泡剂搅拌均匀后，在UV光照射下进行聚合反应，控制聚合起始温度为0-60℃，得到水凝胶；所述复合光引发剂质量为中和液中丙烯酸总量的0.001%-0.3%；所述交联剂质量为中和液中丙烯酸总量的0.01%-0.6%；所述发泡剂质量为中和液中丙烯酸总量的0.01%-3%；
（3）将水凝胶加入切胶造粒机中造粒，造粒过程中均匀加入切胶助剂，制得胶粒，胶粒干燥、粉碎后得初级颗粒；所述切胶助剂的质量为水凝胶质量的2%-15%；
（4）将步骤（3）得到的初级颗粒表面喷涂表面交联液，经热处理后制得最终产品；所述的表面交联液由丙二醇、乙二醇二缩水甘油醚和硫酸盐混合组成，其中丙二醇质量为初级颗粒总质量的0.01-2%；乙二醇二缩水甘油醚质量为初级颗粒总质量的0.005%-0.5%；硫酸盐质量为初级颗粒质量的0.1-4.0%。
2.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（2）中，所述的UV光的波长为150-350nm，光照时间为1-30min。
3.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（2）中，所述复合光引发剂为1-羟基环已基苯基甲酮、2,2-二甲氧基-2-苯基苯乙酮、苯基双(2,4,6-三甲基苯甲酰基)氧化膦、2-苯基苄-2-二甲基胺-1-（4-吗啉苄苯基）丁酮、2-羟基-甲基苯基丙烷-1-酮、双(1-(2,4-二氟苯基)-3-吡咯基)二茂钛、偶氮二异丁醚盐酸盐、二苯基-(2,4,6-三甲基苯甲酰)氧磷、2-甲基-1-(4-甲硫基苯基 )-2-吗啉基-1-丙酮、过硫酸铵、过硫酸钠中的至少一种。
4.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（2）中，所述交联剂为聚乙二醇200、聚乙二醇300、聚乙二醇400、聚乙二醇600、聚乙二醇800、聚乙二醇1000、聚乙二醇1500、聚乙二醇2000、聚乙二醇4000、聚乙二醇6000、聚乙二醇10000、聚乙二醇20000、季戊四醇三丙烯酸酯、季戊四醇三烯丙基醚、二季戊四醇五丙烯酸酯、乙氧化三羟甲基丙烷三丙烯酸酯、1，4-丁二醇二丙烯酸酯;1，6-己二醇二丙烯酸酯、新戊二醇二丙烯酸酯、丙氧基化新戊二醇二丙烯酸酯、乙氧基化新戊二醇二丙烯酸酯、三乙氧基化甘油三丙烯酸酯、乙二醇二缩水甘油醚中的至少一种。
5.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（2）中，所述发泡剂为碳酸氢钠、碳酸氢钾、碳酸氢铵、碳酸钠、碳酸钾、甲苯磺酰肼、4,4-氧代双苯磺酰肼、气相二氧化硅中的至少一种。
6.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（3）中，所述切胶助剂为硬质酸钠、碳酸氢钠、碳酸钠、氢氧化钠、氢氧化钾、蔗糖酯、亚硫酸钠、焦亚硫酸钠中的两种或两种以上。
7.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（3）中胶粒的干燥温度为70-220℃。
8.根据权利要求1所述的具有高抗返渗性能的高吸水性树脂的制备方法，其特征在于：步骤（4）中热处理温度为70-220℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710106337.4A CN106750475B (zh) | 2017-02-27 | 2017-02-27 | 一种具有高抗返渗性能的高吸水性树脂的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710106337.4A CN106750475B (zh) | 2017-02-27 | 2017-02-27 | 一种具有高抗返渗性能的高吸水性树脂的制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106750475A true CN106750475A (zh) | 2017-05-31 |
| CN106750475B CN106750475B (zh) | 2019-08-20 |
Family
ID=58959171
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710106337.4A Active CN106750475B (zh) | 2017-02-27 | 2017-02-27 | 一种具有高抗返渗性能的高吸水性树脂的制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106750475B (zh) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107811760A (zh) * | 2017-11-22 | 2018-03-20 | 上海护理佳实业有限公司 | 一种高吸收奶水的防溢乳垫及其制造方法 |
| CN107857836A (zh) * | 2017-11-22 | 2018-03-30 | 上海护理佳实业有限公司 | 一种高吸收奶水用高吸水树脂及其制造方法 |
| CN108047477A (zh) * | 2017-12-20 | 2018-05-18 | 江苏斯尔邦石化有限公司 | 一种高吸水性树脂的制备方法 |
| CN108610459A (zh) * | 2018-05-22 | 2018-10-02 | 杭州考拉之屋实业有限公司 | 一种快速吸收型高吸水性树脂的制备方法 |
| CN110559124A (zh) * | 2019-08-26 | 2019-12-13 | 广州科莱瑞迪医疗器材股份有限公司 | 一种化疗冰敷袋 |
| CN110746541A (zh) * | 2019-11-05 | 2020-02-04 | 深圳市乐闵科技有限公司 | 一种高耐盐性高吸水性树脂及其制备方法和应用 |
| CN110746532A (zh) * | 2019-11-05 | 2020-02-04 | 深圳市乐闵科技有限公司 | 高抗反渗性的高吸水性树脂及其制备方法和应用 |
| KR20200035860A (ko) * | 2018-09-27 | 2020-04-06 | 주식회사 엘지화학 | 고흡수성 수지 시트의 제조 방법 |
| CN111499914A (zh) * | 2020-04-30 | 2020-08-07 | 江苏斯尔邦石化有限公司 | 一种快吸速型高吸水性树脂的制备方法 |
| EP3677622A4 (en) * | 2018-05-11 | 2020-11-25 | Lg Chem, Ltd. | Process for the production of a superabsorbent polymer layer |
| WO2021071291A1 (ko) * | 2019-10-08 | 2021-04-15 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| KR20210042031A (ko) * | 2019-10-08 | 2021-04-16 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| CN113372611A (zh) * | 2021-06-07 | 2021-09-10 | 万华化学集团股份有限公司 | 一种可提高吸收速度的超吸收聚合物及其制备方法与应用 |
| CN115057957A (zh) * | 2022-08-18 | 2022-09-16 | 山东诺尔生物科技有限公司 | 一种超吸水材料的制备方法及超吸水材料 |
| CN115317247A (zh) * | 2022-07-20 | 2022-11-11 | 浙江卫星新材料科技有限公司 | 一种含有气味轻的高吸收性树脂的纸尿裤 |
| CN116178610A (zh) * | 2022-12-22 | 2023-05-30 | 山东德瑞高分子材料股份有限公司 | 一种高吸水树脂的制备方法 |
| WO2023106878A1 (ko) * | 2021-12-10 | 2023-06-15 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140458A (zh) * | 1994-12-08 | 1997-01-15 | 株式会社日本触媒 | 吸水性树脂及其制造方法以及吸水性树脂组合物 |
| CN102300884A (zh) * | 2009-02-06 | 2011-12-28 | 株式会社日本触媒 | 聚丙烯酸(盐)系吸水性树脂及其制备方法 |
| CN103910896A (zh) * | 2014-04-08 | 2014-07-09 | 万华化学集团股份有限公司 | 一种低返渗高分子吸水树脂的制备方法 |
-
2017
- 2017-02-27 CN CN201710106337.4A patent/CN106750475B/zh active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140458A (zh) * | 1994-12-08 | 1997-01-15 | 株式会社日本触媒 | 吸水性树脂及其制造方法以及吸水性树脂组合物 |
| CN102300884A (zh) * | 2009-02-06 | 2011-12-28 | 株式会社日本触媒 | 聚丙烯酸(盐)系吸水性树脂及其制备方法 |
| CN103910896A (zh) * | 2014-04-08 | 2014-07-09 | 万华化学集团股份有限公司 | 一种低返渗高分子吸水树脂的制备方法 |
Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107811760A (zh) * | 2017-11-22 | 2018-03-20 | 上海护理佳实业有限公司 | 一种高吸收奶水的防溢乳垫及其制造方法 |
| CN107857836A (zh) * | 2017-11-22 | 2018-03-30 | 上海护理佳实业有限公司 | 一种高吸收奶水用高吸水树脂及其制造方法 |
| CN108047477A (zh) * | 2017-12-20 | 2018-05-18 | 江苏斯尔邦石化有限公司 | 一种高吸水性树脂的制备方法 |
| US11278867B2 (en) | 2018-05-11 | 2022-03-22 | Lg Chem, Ltd. | Preparation method for super absorbent polymer sheet |
| EP3677622A4 (en) * | 2018-05-11 | 2020-11-25 | Lg Chem, Ltd. | Process for the production of a superabsorbent polymer layer |
| CN108610459A (zh) * | 2018-05-22 | 2018-10-02 | 杭州考拉之屋实业有限公司 | 一种快速吸收型高吸水性树脂的制备方法 |
| US11773236B2 (en) | 2018-09-27 | 2023-10-03 | Lg Chem, Ltd. | Method of preparing superabsorbent polymer sheet |
| KR102457232B1 (ko) | 2018-09-27 | 2022-10-20 | 주식회사 엘지화학 | 고흡수성 수지 시트의 제조 방법 |
| KR20200035860A (ko) * | 2018-09-27 | 2020-04-06 | 주식회사 엘지화학 | 고흡수성 수지 시트의 제조 방법 |
| EP3680285A4 (en) * | 2018-09-27 | 2020-11-25 | Lg Chem, Ltd. | SUPERABSORBENT POLYMER SHEET MANUFACTURING PROCESS |
| CN110559124A (zh) * | 2019-08-26 | 2019-12-13 | 广州科莱瑞迪医疗器材股份有限公司 | 一种化疗冰敷袋 |
| KR20210042031A (ko) * | 2019-10-08 | 2021-04-16 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| CN114222787B (zh) * | 2019-10-08 | 2023-09-01 | 株式会社Lg化学 | 用于制备超吸收性聚合物的方法 |
| KR102634905B1 (ko) | 2019-10-08 | 2024-02-07 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| CN114222787A (zh) * | 2019-10-08 | 2022-03-22 | 株式会社Lg化学 | 用于制备超吸收性聚合物的方法 |
| WO2021071291A1 (ko) * | 2019-10-08 | 2021-04-15 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| CN110746532B (zh) * | 2019-11-05 | 2022-04-12 | 深圳市乐闵科技有限公司 | 高抗反渗性的高吸水性树脂及其制备方法和应用 |
| CN110746541A (zh) * | 2019-11-05 | 2020-02-04 | 深圳市乐闵科技有限公司 | 一种高耐盐性高吸水性树脂及其制备方法和应用 |
| CN110746532A (zh) * | 2019-11-05 | 2020-02-04 | 深圳市乐闵科技有限公司 | 高抗反渗性的高吸水性树脂及其制备方法和应用 |
| CN111499914A (zh) * | 2020-04-30 | 2020-08-07 | 江苏斯尔邦石化有限公司 | 一种快吸速型高吸水性树脂的制备方法 |
| CN113372611B (zh) * | 2021-06-07 | 2023-12-29 | 万华化学集团股份有限公司 | 一种可提高吸收速度的超吸收聚合物及其制备方法与应用 |
| CN113372611A (zh) * | 2021-06-07 | 2021-09-10 | 万华化学集团股份有限公司 | 一种可提高吸收速度的超吸收聚合物及其制备方法与应用 |
| WO2023106878A1 (ko) * | 2021-12-10 | 2023-06-15 | 주식회사 엘지화학 | 고흡수성 수지의 제조 방법 |
| CN115317247A (zh) * | 2022-07-20 | 2022-11-11 | 浙江卫星新材料科技有限公司 | 一种含有气味轻的高吸收性树脂的纸尿裤 |
| CN115057957A (zh) * | 2022-08-18 | 2022-09-16 | 山东诺尔生物科技有限公司 | 一种超吸水材料的制备方法及超吸水材料 |
| CN116178610A (zh) * | 2022-12-22 | 2023-05-30 | 山东德瑞高分子材料股份有限公司 | 一种高吸水树脂的制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106750475B (zh) | 2019-08-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106750475A (zh) | 一种具有高抗返渗性能的高吸水性树脂的制备方法 | |
| KR100406312B1 (ko) | 개선된성질을가진수분흡수성중합체,그제조방법및용도 | |
| TWI441841B (zh) | 水溶性或水膨脹性聚合物，特別是由丙烯醯胺與至少一離子性共單體所成的低單體殘留量之水溶性或水膨脹性共聚物 | |
| TW434265B (en) | Absorbing agents for water and aqueous liquids and process for their production and use | |
| USRE37021E1 (en) | Water-absorbing resin and process for producing same | |
| US5856410A (en) | Polyacrylate superabsorbent post-polymerization neutralized with solid, non-hydroxyl neutralizing agent. | |
| JP2877255B2 (ja) | 耐久性の優れた吸水性樹脂の製造方法 | |
| CN108047477A (zh) | 一种高吸水性树脂的制备方法 | |
| CN110950993B (zh) | 一种具有低可萃取物含量的丙烯酸吸水树脂制备方法 | |
| CN107987289A (zh) | 一种高温制备聚丙烯酸盐类高吸水性树脂的方法 | |
| CN104744711A (zh) | 一种高白度丙烯酸高吸水树脂及其制备方法 | |
| CN107266617A (zh) | 一种化学引发聚合法生产聚丙烯酸盐类高吸水性树脂的生产方法 | |
| JP3597597B2 (ja) | 吸水性樹脂及びその製造方法 | |
| KR102562511B1 (ko) | 킬레이트제를 포함하는 흡수성 수지의 제조 방법 | |
| JP2018162455A (ja) | 吸水性樹脂の製造方法 | |
| JPH1045812A (ja) | 繊維含有吸水性樹脂の製造方法 | |
| JPH0798847B2 (ja) | 水膨潤性重合体組成物の製造法及び組成物 | |
| CN104650370A (zh) | 吸水树脂及其制备方法 | |
| CN111440338B (zh) | 一种化学引发法制备低可萃取物高吸水性树脂的方法 | |
| JP2012007151A (ja) | 吸収性樹脂の製造方法 | |
| JPH0656933A (ja) | 吸水性樹脂およびその製造方法 | |
| CN109320660A (zh) | 一种医药及高吸水树脂sap生产工艺 | |
| CN111087558A (zh) | 一种改性丙烯酸基高强度耐盐高吸收性树脂及其制备方法 | |
| JP2611786B2 (ja) | 吸水性樹脂の製造法 | |
| CN112011007B (zh) | 可多次吸收的高吸水性树脂及其制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20190725 Address after: 222000 East Gangqian 4th Road and North Lushan 2nd Road, Xuwei New District, Lianyungang City, Jiangsu Province Applicant after: Jiangsu sailboat Petrochemical Co. Ltd. Address before: Room 208, Building 7, Honggang Petrochemical Co., Ltd., Gangqian Avenue, Xuwei New District, Lianyungang City, Jiangsu Province Applicant before: Jiangsu rainbow innovative materials Co. Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |