CN103242468B - Beaded sodium polyacrylate and preparation method thereof - Google Patents
Beaded sodium polyacrylate and preparation method thereof Download PDFInfo
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- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 title claims abstract description 19
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 90
- 229910052757 nitrogen Inorganic materials 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 36
- 239000000178 monomer Substances 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 24
- 229940047670 sodium acrylate Drugs 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 15
- 239000002283 diesel fuel Substances 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 10
- 239000008346 aqueous phase Substances 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 9
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 8
- 239000011118 polyvinyl acetate Substances 0.000 claims description 8
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 6
- 238000010557 suspension polymerization reaction Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000004043 dyeing Methods 0.000 abstract description 2
- 238000007639 printing Methods 0.000 abstract description 2
- 239000004753 textile Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- 238000004090 dissolution Methods 0.000 description 9
- 238000006116 polymerization reaction Methods 0.000 description 9
- 239000003350 kerosene Substances 0.000 description 7
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 4
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 4
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000001856 Ethyl cellulose Substances 0.000 description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229920001249 ethyl cellulose Polymers 0.000 description 3
- 235000019325 ethyl cellulose Nutrition 0.000 description 3
- -1 metallurgy Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000003352 sequestering agent Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000004159 Potassium persulphate Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000003502 gasoline Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- LRDFRRGEGBBSRN-UHFFFAOYSA-N isobutyronitrile Chemical compound CC(C)C#N LRDFRRGEGBBSRN-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 235000019394 potassium persulphate Nutrition 0.000 description 2
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical group CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- KWYJDIUEHHCHCZ-UHFFFAOYSA-N 3-[2-[bis(2-carboxyethyl)amino]ethyl-(2-carboxyethyl)amino]propanoic acid Chemical compound OC(=O)CCN(CCC(O)=O)CCN(CCC(O)=O)CCC(O)=O KWYJDIUEHHCHCZ-UHFFFAOYSA-N 0.000 description 1
- 239000004160 Ammonium persulphate Substances 0.000 description 1
- 108010082495 Dietary Plant Proteins Proteins 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001676573 Minium Species 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 1
- 235000019395 ammonium persulphate Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- FYIBPWZEZWVDQB-UHFFFAOYSA-N dicyclohexyl carbonate Chemical class C1CCCCC1OC(=O)OC1CCCCC1 FYIBPWZEZWVDQB-UHFFFAOYSA-N 0.000 description 1
- ODCCJTMPMUFERV-UHFFFAOYSA-N ditert-butyl carbonate Chemical compound CC(C)(C)OC(=O)OC(C)(C)C ODCCJTMPMUFERV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 230000003019 stabilising effect Effects 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Cosmetics (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention provides beaded sodium polyacrylate (PAANa) and a preparation method thereof. The preparation method is characterized in that an efficient stable system is adopted and an inverse suspension polymerization process is adopted, so that a quick-dissolving PAANa product with high intrinsic viscosity (not less than 10dL/g) and excellent dissolubility (not more than 0.5h) can be prepared. Meanwhile, by adjusting the process, beaded superhigh molecular weight quick-dissolving PAANa products with different intrinsic viscosities can be prepared. The obtained PAANa product can replace aqueous solution type and powdery PAANa products with low intrinsic viscosity, and is expected to be widely applied to water treatment, papermaking, oil exploration, textile printing and dyeing, daily chemical industry and other aspects.
Description
Technical field
The invention belongs to polymers manufacturing field, be specifically related to a kind of pearl sodium polyacrylate and preparation method thereof.
Background technology
Polyacrylic acid and sodium salt thereof are because of the physical and chemical performance of its excellence, there is thickening, suspended dispersed, flocculate, help the effect of washing etc. and be widely used in the aspects such as coating, metallurgy, medicine, makeup, particularly high molecular weight sodium polyacrylate is at foodstuff additive, the flocculation of alumina minium mud, there is unique application the aspects such as the process of animal/vegetable protein waste water.Though aqueous sodium acrylate solution polymerization has advantages such as implementing convenient, equipment simple, product gel content is low, stable system, also exist polymerization later stage viscosity large, stir heat radiation difficulty, be difficult to obtained high molecular weight sodium polyacrylate.U.S. Nalco, Japanese catalyst chemical company adopt belt polymerization technique to solve the difficult problems such as heat transfer, stirring, but equipment manufacturing cost is high, and Controlling Technology is complicated.From the nineties, inverse suspension polymerization process application is polymerized in sodium acrylate by investigator, not only solves the difficult problems such as the high and Stirring heat transfer of viscosity is difficult, and has the large and molecular weight of product advantages of higher of rate of polymerization concurrently, and reaction conditions is gentle, can directly make pearl or powder-like product.But sodium acrylate inverse suspension polymerization process is applied to the production of High hydrophilous resin more at present, the present invention is to prepare the sodium polyacrylate of water-soluble polymer amount for target, the inverse suspension polymerization technique of research sodium acrylate, inquire into stabilising system, water oil ratio, the factors such as stirring velocity are on the impact of polymerization stability, and study the affecting laws of molecular weight regulator to molecular weight, the suitability for industrialized production for the sodium polyacrylate preparing water-soluble polymer amount provides basis.
Summary of the invention
The object of this invention is to provide the preparation method of pearl sodium polyacrylate (PAANa), for meeting the demand in market, the present invention adopts inverse suspension polymerization, control various polymerization process condition, prepare pearl ultra-high molecular weight Instant PAANa product, promote its widespread use in the industries such as coating, food, makeup, tobacco and medicine.
For achieving the above object, the present invention adopts following technical scheme:
(1) sodium acrylate monomers solution allocation: add 300 ~ 400 parts, vinylformic acid in material-compound tank, 400 ~ 600 parts, water, control temperature is 30 ~ 40 DEG C, and slowly dripping concentration is 50% sodium hydroxide solution 300 ~ 400 parts, obtains sodium acrylate monomers solution; Slow dropping is herein understood by those skilled in the art, specifically to make stable reaction and gentleness is as the criterion.In addition, concentration of sodium hydroxide solution is mass concentration.
(2) sodium acrylate monomers solution 200 ~ 350 parts is added respectively at aqueous phase tank; Sequestrant 0.2 ~ 0.6 part; Initiator 2 ~ 5 parts; Azo-initiator 5 ~ 10 parts; Stirring makes it be uniformly dispersed, and obtains monomer phase; Wherein preferred sodium acrylate monomers solution 300 ~ 350 parts; Sequestrant 0.4 ~ 0.5 part; Initiator 3 ~ 4 parts; Azo-initiator 6 ~ 8 parts;
(3) stablizer 4 ~ 8 parts is added in reactor, add hydrocarbon solvent 500 ~ 650 parts simultaneously, then put in the water-bath under room temperature, stir with agitator, simultaneously inflated with nitrogen protection polymerization system under liquid level;
(4) after being filled with 20 ~ 40 minutes nitrogen in reactor, the monomer phase of preparation in temperature of reaction kettle less than 30 ~ 40 DEG C adds step (2), stir 10 ~ 20 minutes, the speed of agitator is 150 ~ 200r/min, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen;
(5) slowly temperature is raised to 60 ~ 70 DEG C, answers 2 ~ 3 hours, after reaction terminates, stop filling nitrogen, distill after being warmed up to 80 ~ 90 DEG C, distillation time 1 ~ 2 hour;
(6) after having distilled, product is sent into drying machine drying, packing and storing after dry.
Method of the present invention, described sequestrant is one or more in EDTA, Sodium Dimercapto Sulfonate, EGTA, ethylenediamine tetrapropionic acid(EDTP), triethylenetetramine.
Method of the present invention, described stablizer is macromolecular compound that is natural and/or synthesis, and it consists of the multipolymer of hydroxypropylcellulose, ethyl cellulose, Polyvinylpyrolidone (PVP), polyvinyl acetate, polymethyl acrylic acid, polyvinyl alcohol, vinylbenzene and maleic anhydride one or more; Preferred polyvinyl acetate: polymethyl acrylic acid is the mixture of 1:1.
Method of the present invention, described hydrocarbon solvent is selected from one or more in gasoline, kerosene, diesel oil or white oil.Be preferably kerosene and diesel oil 1:1 mixture.
Method of the present invention, described initiator is selected from Potassium Persulphate, Sodium Persulfate, ammonium persulphate, benzoyl peroxide, lauroyl peroxide, cross two carbonic acid dicyclohexyl esters, cross octanoic acid ter-butyl ester, cross sad tert-pentyl ester, cross in nonane diacid di tert butyl carbonate, t-butyl peroxy-acetate one or more.
Method of the present invention, described azo-initiator is selected from Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-iso-dimethyl, 2,2 '-azo two (isopropyl cyanide), 2, one or more in 2 '-azo two (2-methyliso-butyronitrile).Be preferably 2,2'-Azobis(2,4-dimethylvaleronitrile).
Method of the present invention, in step 3, stirring velocity is 50 ~ 100r/min, and churning time is 5 minutes.Under this agitation condition, monomer can be uniformly dispersed mutually.
Method of the present invention, in described step 6, drying temperature is 90 ~ 120 DEG C, and time of drying is 2 ~ 3 hours.
Method of the present invention, described drying machine is selected from cylindrical drier, cascade type dryer, boiling laminar drying machine or spiral dryer.
As a kind of preferred forms of the present invention, preferably described preparation method comprises the steps:
(1) configure sodium acrylate monomers solution: in material-compound tank, add 350 parts, vinylformic acid, 500 parts, water, control temperature is 35 DEG C, slowly drip 50% sodium hydroxide solution 350 parts;
(2) sodium acrylate monomers solution 250 parts is added respectively at aqueous phase tank; EDTA0.4 part; Benzoyl peroxide 3.5 parts; Azo-bis-iso-dimethyl initiator 8 parts; Stirring and dissolving is uniformly dispersed, and obtains monomer phase;
(3) be that the stablizer 6 parts of 1:1 adds in reactor by polyvinyl acetate and polymethyl acrylic acid mass ratio, add diesel oil 550 parts simultaneously, then put in the water-bath under room temperature, stir with agitator, under liquid level, be filled with nitrogen simultaneously;
(4) after being filled with 30 minutes nitrogen in reactor, adding monomer stir 15 minutes mutually temperature of reaction kettle less than 35 DEG C, the speed of agitator is 180r/min, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen;
(5) slowly temperature is raised to 70 DEG C, reacts 2.5 hours, stop filling nitrogen, start distillation after being warmed up to 85 DEG C, distillation time is 1.5 hours;
(6) after having distilled, product is sent into drying machine drying, drying temperature is 100 DEG C, and drying time is 2.5 hours, packing and storing after dry.
In addition, the pearl sodium polyacrylate (PAANa) obtained by the further claimed above-mentioned preparation method of the present invention.
The key of the technology of the present invention is the use of efficient stable system, adopts anti-phase suspension emulsion polymerization technique, can prepare limiting viscosity high (>=10dL/g), Instant pearl sodium polyacrylate (the being called for short PAANa) product of solvability splendid (≤0.5h).Meanwhile, by adjusting process, the pearl ultra-high molecular weight Instant PAANa product of different qualities viscosity can be prepared.The PAANa product of aqueous solution type and the low limiting viscosity of powdery can be substituted, will be used widely in water treatment, papermaking, oil production, textile printing and dyeing and daily-use chemical industry etc.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.If do not specialize, the conventional means that technique means used in embodiment is well known to those skilled in the art, is raw materials usedly commercial goods.
Embodiment 1
A preparation method for pearl sodium polyacrylate, comprises the steps:
(1) configuration of sodium acrylate monomers solution: add vinylformic acid 330g in material-compound tank, water 450g, control temperature is 36 DEG C, slowly drips 50% sodium hydroxide solution 310g; (2) sodium acrylate monomers solution 300 parts is added respectively at aqueous phase tank; EDTA0.5g; Benzoyl peroxide 3g; Azo-bis-iso-dimethyl 6g; Stirring and dissolving is uniformly dispersed, and obtains single-phase body.
(3) the stablizer 5g being 1:1 by polyvinyl acetate and polymethyl acrylic acid mass ratio adds in reactor, then add diesel oil and kerosene mass ratio is 1:1 mixed solvent 600g, be then incubated 30 DEG C, stir with agitator, stirring velocity is 100r/min, simultaneously inflated with nitrogen under liquid level.
(4) after being filled with 30 minutes nitrogen in reactor, adding monomer stir 10 minutes mutually temperature of reaction kettle less than 30 DEG C, the speed of agitator is 160r/min, nitrogen tube to be adjusted on liquid level and to continue to fill nitrogen.
(5) slowly temperature is risen 70 DEG C of reactions 2 hours, after reaction terminates, stop filling nitrogen; Heat up after 85 DEG C and start distillation.After having distilled, it is dry that product sends into drying machine, and drying temperature is 100 DEG C, and time of drying is 2.5 hours.Obtaining product performance viscosity number is 12.36dl/g; Dissolution time is 25min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 400um
Embodiment 2:
A preparation method for pearl sodium polyacrylate, comprises the steps:
(1) configuration of sodium acrylate monomers solution: add vinylformic acid 360g in material-compound tank, water 500g, control temperature is 40 DEG C, slowly drips 50% sodium hydroxide solution 350g;
(2) sodium acrylate monomers solution 300g is added respectively at aqueous phase tank; EDTA0.4g; Benzoyl peroxide 3g; 2,2'-Azobis(2,4-dimethylvaleronitrile) 8g; Stirring and dissolving is uniformly dispersed, and obtains single-phase body.
(3) the stablizer 6g being 1:1 by polyvinyl acetate and hydroxypropylcellulose mass ratio adds in reactor, then adds diesel oil and kerosene mass ratio is 1:1 mixed solvent 600g, is then incubated 30 DEG C, stirs with agitator, is filled with nitrogen under liquid level simultaneously.
(4) after being filled with 30 minutes nitrogen in reactor, adding monomer temperature of reaction kettle less than 30 DEG C and stir 15 minutes mutually, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen.
(5) slowly temperature is risen 70 DEG C of reactions 2.5 hours, after reaction terminates, stop filling nitrogen, heats up after 85 DEG C and start to distill, the time of distillation regulates as required.After having distilled, it is dry that product sends into drying machine, and drying temperature is 90 DEG C, and time of drying is 3 hours.Obtaining product performance viscosity number is 11.24dl/g; Dissolution time is 22min, and median size is 350um pearl ultra-high molecular weight Instant PAANa product.
Embodiment 3
A preparation method for pearl sodium polyacrylate, comprises the steps:
(1) configuration of sodium acrylate monomers solution: add vinylformic acid 350g in material-compound tank, water 500g, control temperature is 35 DEG C, slowly drips 50% sodium hydroxide solution 320g;
(2) sodium acrylate monomers solution 300g is added respectively at aqueous phase tank; EGTA0.5g; Benzoyl peroxide 4g; Azo-bis-iso-dimethyl 6g; Stirring and dissolving is uniformly dispersed.
(3) the stablizer 4g being 1:1 by polyvinyl acetate and Polyvinylpyrolidone (PVP) mass ratio adds in reactor; then diesel oil is added and kerosene mass ratio is 1:1 mixed solvent 600g; then 30 DEG C are incubated; stir with agitator; stirring velocity is 100 turns, is filled with nitrogen protection polymerization system under liquid level simultaneously.
(4) after being filled with 20 minutes nitrogen in reactor, adding monomer stir 10 minutes mutually temperature of reaction kettle less than 30 DEG C, the speed of agitator is 160r/min, nitrogen tube is adjusted on liquid level and continues inflated with nitrogen.
(5) slowly temperature is risen 66 DEG C of reactions 2 hours, reaction terminates rear stopping and filling nitrogen, and heats up after 85 DEG C and start to distill, the time of distillation regulates as required.After having distilled, it is dry that product sends into drying machine, and drying temperature is 120 DEG C, and time of drying is 2 hours.Obtaining product performance viscosity number is 11.52dl/g; Dissolution time is 18min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 600um
Embodiment 4
A preparation method for pearl sodium polyacrylate, comprises the steps:
(1) configuration of sodium acrylate monomers solution: add vinylformic acid 300g in material-compound tank, water 400g, control temperature is 30 DEG C, slowly drips 50% sodium hydroxide solution 300g;
(2) sodium acrylate monomers solution 300g is added respectively at aqueous phase tank; EDTA0.5g; Lauroyl peroxide 3g; Diisopropyl azodicarboxylate 5g; Stirring and dissolving is uniformly dispersed, and obtains single-phase body.
(3) the stablizer 5g being 1:1 by ethyl cellulose and polymethyl acrylic acid mass ratio adds in reactor; then diesel oil is added and kerosene mass ratio is 1:1 mixed solvent 600g; then 30 DEG C are incubated; stir with agitator; stirring velocity is 100 turns, is filled with nitrogen protection polymerization system under liquid level simultaneously.
(4) after being filled with 20 minutes nitrogen in reactor, adding monomer stir 10 minutes mutually temperature of reaction kettle less than 30 DEG C, the speed of agitator is 160r/min, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen.
(5) slowly temperature is risen 68 DEG C of reactions 2 hours, reaction terminates rear stopping and filling nitrogen, and heats up after 85 DEG C and start to distill, the time of distillation regulates as required.After having distilled, it is dry that product sends into drying machine, and drying temperature is 110 DEG C, and time of drying is 2 hours.Obtaining product performance viscosity number is 12.66dl/g; Dissolution time is 25min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 400um
Embodiment 5
A preparation method for pearl sodium polyacrylate, comprises the steps:
(1) configuration of sodium acrylate monomers solution: add vinylformic acid 400g in material-compound tank, water 600g, control temperature is 40 DEG C, slowly drips 50% sodium hydroxide solution 400g;
(2) sodium acrylate monomers solution 320g is added respectively at aqueous phase tank; EDTA0.5g; Benzoyl peroxide 3g; Azo-bis-iso-dimethyl 6g; Stirring and dissolving is uniformly dispersed, and obtains single-phase body.
(3) the stablizer 6g being 1:1 by hydroxypropylcellulose and Polyvinylpyrolidone (PVP) mass ratio adds in reactor; then diesel oil is added and kerosene mass ratio is 1:1 mixed solvent 600g; then 30 DEG C are incubated; stir with agitator; stirring velocity is 100 turns, is filled with nitrogen protection polymerization system under liquid level simultaneously.
(4) after being filled with 20 minutes nitrogen in reactor, adding monomer stir 10 minutes mutually temperature of reaction kettle less than 30 DEG C, the speed of agitator is 160r/min, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen.
(5) slowly temperature is risen 70 DEG C of reactions 2 hours, after reaction terminates, stop filling nitrogen, heats up after 85 DEG C and start to distill, the time of distillation regulates as required.After having distilled, it is dry that product sends into drying machine, and drying temperature is 110 DEG C, and time of drying is 2 hours.Obtaining product performance viscosity number is 13.22dl/g; Dissolution time is 25min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 350um.
Embodiment 6
A preparation method for pearl sodium polyacrylate, comprises the steps:
(1) configure sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 350g, water 500g, control temperature is 35 DEG C, slowly drip 50% sodium hydroxide solution 350g;
(2) sodium acrylate monomers solution 250g is added respectively at aqueous phase tank; EDTA0.4g; Benzoyl peroxide 3.5g; Initiator azo-bis-iso-dimethyl 8g; Stirring and dissolving is uniformly dispersed, and obtains monomer phase;
(3) the stablizer 6g being 1:1 by polyvinyl acetate and polymethyl acrylic acid mass ratio adds in reactor, adds diesel oil 550g simultaneously, then puts in the water-bath under room temperature, stirs with agitator, is filled with nitrogen under liquid level simultaneously;
(4) after being filled with 30 minutes nitrogen in reactor, adding monomer stir 15 minutes mutually temperature of reaction kettle less than 35 DEG C, the speed of agitator is 180r/min, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen;
(5) slowly temperature is raised to 70 DEG C, reacts 2.5 hours, stop filling nitrogen, start distillation after being warmed up to 85 DEG C, distillation time is 1.5 hours;
(6) after having distilled, product is sent into drying machine drying, drying temperature is 100 DEG C, and drying time is 2.5 hours.Obtaining product performance viscosity number is 13.88dl/g; Dissolution time is 21min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 450um.
Embodiment 7
Compared with embodiment 1, the difference of the present embodiment is only that stability is hydroxypropylcellulose: ethyl cellulose is by the mixture of 1:1; Described organic solvent is white oil; Initiator is Potassium Persulphate, azo-initiator is 2,2 '-azo two (2-methyliso-butyronitrile).Obtaining product performance viscosity number is 12.28dl/g; Dissolution time is 24min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 400um.
Embodiment 8
Compared with embodiment 7, the difference of the present embodiment is only that stability is polyvinyl alcohol; Described organic solvent is diesel oil; Initiator was sad tert-pentyl ester, azo-initiator is 2,2 '-azo two (isopropyl cyanide).Obtaining product performance viscosity number is 12.25dl/g; Dissolution time is 25min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 400um.
Embodiment 9
Compared with embodiment 7, the difference of the present embodiment is only that stability is Polyvinylpyrolidone (PVP); Described organic solvent is gasoline: diesel oil is the mixture of 1:1; Initiator is t-butyl peroxy-acetate, azo-initiator is 2,2'-Azobis(2,4-dimethylvaleronitrile).Obtaining product performance viscosity number is 12.23dl/g; Dissolution time is 26min, and median size is the pearl ultra-high molecular weight Instant PAANa product of 400um.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (2)
1. a preparation method for pearl sodium polyacrylate, is characterized in that: comprise the steps:
(1) configure sodium acrylate monomers solution: in material-compound tank, add 350 parts, vinylformic acid, 500 parts, water, control temperature is 35 DEG C, slowly drip 350 parts, sodium hydroxide;
(2) sodium acrylate monomers solution 250 parts is added respectively at aqueous phase tank; EDTA0.4 part; Benzoyl peroxide 3.5 parts; Initiator azo-bis-iso-dimethyl 8 parts; Stirring and dissolving is uniformly dispersed, and obtains monomer phase;
(3) be that the stablizer 6 parts of 1:1 adds in reactor by polyvinyl acetate and polymethyl acrylic acid mass ratio, add diesel oil 550 parts simultaneously, then put in the water-bath under room temperature, stir with agitator, under liquid level, be filled with nitrogen simultaneously;
(4) after being filled with 30 minutes nitrogen in reactor, adding monomer stir 15 minutes mutually temperature of reaction kettle less than 35 DEG C, the speed of agitator is 180r/min, nitrogen tube to be adjusted on liquid level and to continue inflated with nitrogen;
(5) slowly temperature is raised to 70 DEG C, reacts 2.5 hours, stop filling nitrogen, start distillation after being warmed up to 85 DEG C, distillation time is 1.5 hours;
(6) after having distilled, product is sent into drying machine drying, drying temperature is 100 DEG C, and drying time is 2.5 hours, packing and storing after dry.
2. the pearl sodium polyacrylate described in claim 1 obtained by preparation method.
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| CN105296437B (en) * | 2015-07-03 | 2019-01-04 | 上海诺百生物科技有限公司 | A kind of slow virus method for concentration |
| CN105949361B (en) * | 2016-06-15 | 2018-04-13 | 湖州超能生化有限公司 | A kind of preparation method of solid-state Sodium Polyacrylate |
| CN106699936B (en) * | 2016-12-01 | 2018-02-27 | 湖北硅金凝节能减排科技有限公司 | A kind of preparation method of high molecular weight sodium polyacrylate |
| CN108003856B (en) * | 2017-12-01 | 2020-07-07 | 北京恒聚化工集团有限责任公司 | Beaded microsphere profile control water shutoff agent and preparation method thereof |
| CN109369833A (en) * | 2018-10-26 | 2019-02-22 | 江门市新会区中盛生物科技有限公司 | A method of Sodium Polyacrylate is prepared by ternary initiator system |
| CN110465619B (en) * | 2019-08-02 | 2021-03-19 | 宁夏共享化工有限公司 | Sodium polyacrylate binder system for casting and preparation method thereof |
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