CN103242468A - Beaded sodium polyacrylate and preparation method thereof - Google Patents
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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 polymkeric substance and make the 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 its excellent physical chemistry, have thickening, suspended dispersed, flocculate, help effect such as wash and be widely used in aspects such as coating, metallurgy, medicine, makeup, particularly high molecular weight sodium polyacrylate is at foodstuff additive, the flocculation of alumina minium mud, the aspects such as processing of animal/vegetable protein waste water have unique application.Implement advantages such as convenient, that equipment is simple, the product gel content is low, system is stable though the sodium acrylate aqueous solution polymerization has, exist polymerization later stage viscosity big, stir the heat radiation difficulty, be difficult to make high molecular weight sodium polyacrylate.U.S. Nalco, Japanese catalyst chemical company adopt the belt polymerization technique to solve difficult problems such as heat transfer, stirring, but the equipment manufacturing cost height, the control complex process.Since the nineties, the investigator in the sodium acrylate polymerization, has not only solved difficult problems such as viscosity height and Stirring heat transfer difficulty with the inverse suspension polymerization process application, and has the big and molecular weight of product advantages of higher of rate of polymerization concurrently, and the reaction conditions gentleness can directly be made pearl or powder-like product.But sodium acrylate inverse suspension polymerization technology is applied to the production of High hydrophilous resin more at present, the present invention is target with the sodium polyacrylate of preparation water-soluble polymer amount, the inverse suspension polymerization technology of research sodium acrylate, inquire into stabilising system, water oil ratio, factors such as stirring velocity are to the influence of polymerization stability, and the research molecular weight regulator is to the rule that influences of molecular weight, for the suitability for industrialized production of the sodium polyacrylate of preparation water-soluble polymer amount provides the basis.
Summary of the invention
The preparation method who the purpose of this invention is to provide pearl sodium polyacrylate (PAANa), for satisfying the demand in market, the present invention adopts inverse suspension polymerization, control various polymerization process conditions, prepare the instant type PAANa product of pearl ultra-high molecular weight, promoted its widespread use in 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: in material-compound tank, add 300～400 parts in vinylformic acid, 400～600 parts in water, the control temperature is 30～40 ℃, slowly dripping concentration is 300～400 parts of 50% sodium hydroxide solutions, obtains sodium acrylate monomers solution; Slow dropping is herein understood by those skilled in the art, and concrete so that stable reaction and gentleness are as the criterion.In addition, concentration of sodium hydroxide solution is mass concentration.
(2) add 200～350 parts of sodium acrylate monomers solution respectively at the water jar; 0.2～0.6 part of sequestrant; 2～5 parts of initiators; 5～10 parts of azo-initiators; Stirring is uniformly dispersed it, gets the monomer phase; Wherein preferred sodium acrylate monomers solution is 300～350 parts; 0.4～0.5 part of sequestrant; 3～4 parts of initiators; 6～8 parts of azo-initiators;
(3) with in 4～8 parts of adding reactors of stablizer, add 500～650 parts of organic hydrocarbon solvents simultaneously, put into then in the water-bath under the room temperature, stir with agitator, simultaneously inflated with nitrogen protection polymerization system under liquid level;
(4) charge into 20～40 minutes nitrogen in the reactor after, add the monomer phase for preparing in the step (2) below 30～40 ℃ at temperature of reaction kettle, stirred 10～20 minutes, the speed of agitator is 150～200r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen;
(5) slowly temperature is raised to 60～70 ℃, answered 2～3 hours, after reaction finishes, stop to fill nitrogen, be warmed up to 80～90 ℃ after distillation, distillation time 1～2 hour;
(6) after distillation is finished, product is sent into the drying machine drying, dry back packing and storing.
Method of the present invention, described sequestrant are one or more in EDTA, Sodium Dimercapto Sulfonate, EGTA, ethylenediamine tetrapropionic acid(EDTP), the triethylenetetramine.
Method of the present invention, described stablizer is natural and/or synthetic macromolecular compound, and it consists of one or more of multipolymer of hydroxypropylcellulose, ethyl cellulose, Polyvinylpyrolidone (PVP), polyvinyl acetate, polymethyl acrylic acid, polyvinyl alcohol, vinylbenzene and maleic anhydride; Preferred polyvinyl acetate: polymethyl acrylic acid is the mixture of 1:1.
Method of the present invention, described organic hydrocarbon solvent is selected from one or more in gasoline, kerosene, diesel oil or the white oil.Be preferably kerosene and diesel oil 1:1 mixture.
Method of the present invention, described initiator be selected from Potassium Persulphate, Sodium Persulfate, ammonium persulphate, benzoyl peroxide, lauroyl peroxide, cross two carbonic acid dicyclohexyl esters, cross the sad tert-butyl ester, cross sad tert-pentyl ester, cross in nonane diacid di tert butyl carbonate, the 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 cyanides), 2,2 '-in the azo two (2-methyl isopropyl cyanide) one or more.Be preferably 2,2'-Azobis(2,4-dimethylvaleronitrile).
Method of the present invention, in the step 3, stirring velocity is 50～100r/min, churning time is 5 minutes.Under this agitation condition, monomer can be uniformly dispersed mutually.
Method of the present invention, drying temperature is 90～120 ℃ in the described step 6, be 2～3 hours time of drying.
Method of the present invention, described drying machine are selected from cylindrical drier, cascade type dryer, boiling laminar drying machine or spiral drying machine.
As a kind of preferred forms of the present invention, preferred described preparation method comprises the steps:
(1) configuration sodium acrylate monomers solution: in material-compound tank, add 350 parts in vinylformic acid, 500 parts in water, the control temperature is 35 ℃, slowly Dropwise 5 0% sodium hydroxide solution is 350 parts;
(2) add 250 parts of sodium acrylate monomers solution respectively at the water jar; EDTA0.4 part; 3.5 parts of benzoyl peroxides; 8 parts of azo-bis-iso-dimethyl initiators; Stirring and dissolving is uniformly dispersed, and gets the monomer phase;
(3) be in 6 parts of adding reactors of stablizer of 1:1 with polyvinyl acetate and polymethyl acrylic acid mass ratio, add 550 parts of diesel oil simultaneously, put into then in the water-bath under the room temperature, stir with agitator, under liquid level, charge into nitrogen simultaneously;
(4) charge into 30 minutes nitrogen in the reactor after, add monomer below 35 ℃ at temperature of reaction kettle and stirred mutually 15 minutes, the speed of agitator is 180r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen;
(5) slowly temperature is raised to 70 ℃, reacted 2.5 hours, stop to fill nitrogen, begin distillation after being warmed up to 85 ℃, distillation time is 1.5 hours;
(6) after distillation is finished, product is sent into the drying machine drying, drying temperature is 100 ℃, and drying time is 2.5 hours, dry back packing and storing.
In addition, the further prepared pearl sodium polyacrylate of claimed above-mentioned preparation method (PAANa) of the present invention.
The key of the technology of the present invention has been to use the efficient stable system, adopts the anti-phase suspension emulsion polymerization technique, can prepare the limiting viscosity height (〉=10dL/g), splendid (≤0.5h) instant type pearl sodium polyacrylate (the being called for short PAANa) product of solvability.Simultaneously, by adjusting process, can prepare the instant type PAANa product of pearl ultra-high molecular weight of different qualities viscosity.Can the place of water solution-type and the PAANa product of the low limiting viscosity of powdery, will be used widely at aspects such as water treatment, papermaking, oil production, textile printing and dyeing and daily-use chemical industries.
Embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.If do not specialize the conventional means that used technique means is well known to those skilled in the art among the embodiment, the raw materials used commercial goods that is.
Embodiment 1
A kind of preparation method of pearl sodium polyacrylate comprises the steps:
(1) configuration of sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 330g, water 450g, the control temperature is 36 ℃, slowly Dropwise 5 0% sodium hydroxide solution 310g; (2) add 300 parts of sodium acrylate monomers solution respectively at the water jar; EDTA0.5g; Benzoyl peroxide 3g; Azo-bis-iso-dimethyl 6g; Stirring and dissolving is uniformly dispersed, and gets single-phase body.
(3) be in the stablizer 5g adding reactor of 1:1 with polyvinyl acetate and polymethyl acrylic acid mass ratio, adding diesel oil and kerosene mass ratio then is 1:1 mixed solvent 600g, is incubated 30 ℃ then, stirs with agitator, stirring velocity is 100r/min, simultaneously inflated with nitrogen under liquid level.
(4) charge into 30 minutes nitrogen in the reactor after, add monomer below 30 ℃ at temperature of reaction kettle and stirred mutually 10 minutes, the speed of agitator is 160r/min, is adjusted to nitrogen tube on the liquid level and continues to fill nitrogen.
(5) slowly temperature is risen 70 ℃ of reactions 2 hours, reaction stops to fill nitrogen after finishing; Heat up and begin distillation after 85 ℃.After distillation was finished, product was sent into the drying machine drying, and drying temperature is 100 ℃, and be 2.5 hours time of drying.Obtaining the product performance viscosity number is 12.36dl/g; Dissolution time is 25min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 400um
Embodiment 2:
A kind of preparation method of pearl sodium polyacrylate comprises the steps:
(1) configuration of sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 360g, water 500g, the control temperature is 40 ℃, slowly Dropwise 5 0% sodium hydroxide solution 350g;
(2) add sodium acrylate monomers solution 300g respectively at the water jar; EDTA0.4g; Benzoyl peroxide 3g; 2,2'-Azobis(2,4-dimethylvaleronitrile) 8g; Stirring and dissolving is uniformly dispersed, and gets single-phase body.
(3) be that adding diesel oil and kerosene mass ratio then is 1:1 mixed solvent 600g, is incubated 30 ℃ then, stirs with agitator, charges into nitrogen simultaneously under liquid level in the stablizer 6g adding reactor of 1:1 with polyvinyl acetate and hydroxypropylcellulose mass ratio.
(4) charge into 30 minutes nitrogen in the reactor after, add monomer below 30 ℃ at temperature of reaction kettle and stirred mutually 15 minutes, be adjusted to nitrogen tube on the liquid level and continue inflated with nitrogen.
(5) slowly temperature is risen 70 ℃ of reactions 2.5 hours, reaction stops to fill nitrogen after finishing, and heats up to begin to distill after 85 ℃, and the time of distillation is regulated as required.After distillation was finished, product was sent into the drying machine drying, and drying temperature is 90 ℃, and be 3 hours time of drying.Obtaining the product performance viscosity number is 11.24dl/g; Dissolution time is 22min, and median size is the instant type PAANa product of 350um pearl ultra-high molecular weight.
Embodiment 3
A kind of preparation method of pearl sodium polyacrylate comprises the steps:
(1) configuration of sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 350g, water 500g, the control temperature is 35 ℃, slowly Dropwise 5 0% sodium hydroxide solution 320g;
(2) add sodium acrylate monomers solution 300g respectively at the water jar; EGTA0.5g; Benzoyl peroxide 4g; Azo-bis-iso-dimethyl 6g; Stirring and dissolving is uniformly dispersed.
(3) be in the stablizer 4g adding reactor of 1:1 with polyvinyl acetate and Polyvinylpyrolidone (PVP) mass ratio; adding diesel oil and kerosene mass ratio then is 1:1 mixed solvent 600g; be incubated 30 ℃ then; stir with agitator; stirring velocity is 100 commentaries on classics, charges into the nitrogen protection polymerization system simultaneously under liquid level.
(4) charge into 20 minutes nitrogen in the reactor after, add monomer below 30 ℃ at temperature of reaction kettle and stirred mutually 10 minutes, the speed of agitator is 160r/min, nitrogen tube is adjusted to continues inflated with nitrogen on the liquid level.
(5) slowly temperature is risen 66 ℃ of reactions 2 hours, reaction stops to fill nitrogen after finishing, and heats up to begin to distill after 85 ℃, and the time of distillation is regulated as required.After distillation was finished, product was sent into the drying machine drying, and drying temperature is 120 ℃, and be 2 hours time of drying.Obtaining the product performance viscosity number is 11.52dl/g; Dissolution time is 18min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 600um
Embodiment 4
A kind of preparation method of pearl sodium polyacrylate comprises the steps:
(1) configuration of sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 300g, water 400g, the control temperature is 30 ℃, slowly Dropwise 5 0% sodium hydroxide solution 300g;
(2) add sodium acrylate monomers solution 300g respectively at the water jar; EDTA0.5g; Lauroyl peroxide 3g; Diisopropyl azodicarboxylate 5g; Stirring and dissolving is uniformly dispersed, and gets single-phase body.
(3) be in the stablizer 5g adding reactor of 1:1 with ethyl cellulose and polymethyl acrylic acid mass ratio; adding diesel oil and kerosene mass ratio then is 1:1 mixed solvent 600g; be incubated 30 ℃ then; stir with agitator; stirring velocity is 100 commentaries on classics, charges into the nitrogen protection polymerization system simultaneously under liquid level.
(4) charge into 20 minutes nitrogen in the reactor after, add monomer below 30 ℃ at temperature of reaction kettle and stirred mutually 10 minutes, the speed of agitator is 160r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen.
(5) slowly temperature is risen 68 ℃ of reactions 2 hours, reaction stops to fill nitrogen after finishing, and heats up to begin to distill after 85 ℃, and the time of distillation is regulated as required.After distillation was finished, product was sent into the drying machine drying, and drying temperature is 110 ℃, and be 2 hours time of drying.Obtaining the product performance viscosity number is 12.66dl/g; Dissolution time is 25min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 400um
Embodiment 5
A kind of preparation method of pearl sodium polyacrylate comprises the steps:
(1) configuration of sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 400g, water 600g, the control temperature is 40 ℃, slowly Dropwise 5 0% sodium hydroxide solution 400g;
(2) add sodium acrylate monomers solution 320g respectively at the water jar; EDTA0.5g; Benzoyl peroxide 3g; Azo-bis-iso-dimethyl 6g; Stirring and dissolving is uniformly dispersed, and gets single-phase body.
(3) be in the stablizer 6g adding reactor of 1:1 with hydroxypropylcellulose and Polyvinylpyrolidone (PVP) mass ratio; adding diesel oil and kerosene mass ratio then is 1:1 mixed solvent 600g; be incubated 30 ℃ then; stir with agitator; stirring velocity is 100 commentaries on classics, charges into the nitrogen protection polymerization system simultaneously under liquid level.
(4) charge into 20 minutes nitrogen in the reactor after, add monomer below 30 ℃ at temperature of reaction kettle and stirred mutually 10 minutes, the speed of agitator is 160r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen.
(5) slowly temperature is risen 70 ℃ of reactions 2 hours, reaction stops to fill nitrogen after finishing, and heats up to begin to distill after 85 ℃, and the time of distillation is regulated as required.After distillation was finished, product was sent into the drying machine drying, and drying temperature is 110 ℃, and be 2 hours time of drying.Obtaining the product performance viscosity number is 13.22dl/g; Dissolution time is 25min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 350um.
Embodiment 6
A kind of preparation method of pearl sodium polyacrylate comprises the steps:
(1) configuration sodium acrylate monomers solution: in material-compound tank, add vinylformic acid 350g, water 500g, the control temperature is 35 ℃, slowly Dropwise 5 0% sodium hydroxide solution 350g;
(2) add sodium acrylate monomers solution 250g respectively at the water jar; EDTA0.4g; Benzoyl peroxide 3.5g; Initiator azo-bis-iso-dimethyl 8g; Stirring and dissolving is uniformly dispersed, and gets the monomer phase;
(3) be in the stablizer 6g adding reactor of 1:1 with polyvinyl acetate and polymethyl acrylic acid mass ratio, add diesel oil 550g simultaneously, put into then in the water-bath under the room temperature, stir with agitator, under liquid level, charge into nitrogen simultaneously;
(4) charge into 30 minutes nitrogen in the reactor after, add monomer below 35 ℃ at temperature of reaction kettle and stirred mutually 15 minutes, the speed of agitator is 180r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen;
(5) slowly temperature is raised to 70 ℃, reacted 2.5 hours, stop to fill nitrogen, begin distillation after being warmed up to 85 ℃, distillation time is 1.5 hours;
(6) after distillation is finished, product is sent into the drying machine drying, drying temperature is 100 ℃, and drying time is 2.5 hours.Obtaining the product performance viscosity number is 13.88dl/g; Dissolution time is 21min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 450um.
Embodiment 7
Compare with embodiment 1, the difference of present embodiment only is that stability is hydroxypropylcellulose: ethyl cellulose is pressed the mixture of 1:1; Described organic solvent is white oil; Initiator be Potassium Persulphate, azo-initiator be 2,2 '-azo two (2-methyl isopropyl cyanide).Obtaining the product performance viscosity number is 12.28dl/g; Dissolution time is 24min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 400um.
Embodiment 8
Compare with embodiment 7, the difference of present embodiment only is that stability is polyvinyl alcohol; Described organic solvent is diesel oil; Initiator be sad tert-pentyl ester, azo-initiator be 2,2 '-azo two (isopropyl cyanide).Obtaining the product performance viscosity number is 12.25dl/g; Dissolution time is 25min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 400um.
Embodiment 9
Compare with embodiment 7, the difference of present embodiment only is that stability is Polyvinylpyrolidone (PVP); Described organic solvent is gasoline: diesel oil is the mixture of 1:1; Initiator is that t-butyl peroxy-acetate, azo-initiator are 2,2'-Azobis(2,4-dimethylvaleronitrile).Obtaining the product performance viscosity number is 12.23dl/g; Dissolution time is 26min, and median size is the instant type PAANa product of the pearl ultra-high molecular weight of 400um.
Though 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 all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. the preparation method of a pearl sodium polyacrylate is characterized in that: comprise the steps:
(1) sodium acrylate monomers solution allocation: in material-compound tank, add 300～400 parts in vinylformic acid, 400～600 parts in water, the control temperature is 30～40 ℃, slowly dripping concentration is 300～400 parts of 50% sodium hydroxide solutions, obtains sodium acrylate monomers solution;
(2) add 200～350 parts of sodium acrylate monomers solution respectively at the water jar; 0.2～0.6 part of sequestrant; 2～5 parts of initiators; 5～10 parts of azo-initiators; Stirring is uniformly dispersed it, gets the monomer phase;
(3) with in 4～8 parts of adding reactors of stablizer, add 500～650 parts of organic hydrocarbon solvents simultaneously, put into then in the water-bath under the room temperature, stir with agitator, under liquid level, charge into the nitrogen protection polymerization system simultaneously;
(4) charge into 20～40 minutes nitrogen in the reactor after, add the monomer phase for preparing in the step (2) below 30～40 ℃ at temperature of reaction kettle, stirred 10～20 minutes, the speed of agitator is 150～200r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen protection polymerization system;
(5) slowly temperature is raised to 60～70 ℃ and answered 2～3 hours, after reaction finishes, stop to fill nitrogen, be warmed up to 80～90 ℃ after distillation, distillation time 1～2 hour;
(6) after distillation is finished, product is sent into the drying machine drying, dry back packing and storing.
2. preparation method according to claim 1, it is characterized in that: described sequestrant is one or more in EDTA, Sodium Dimercapto Sulfonate, EGTA, ethylenediamine tetrapropionic acid(EDTP), the triethylenetetramine.
3. preparation method according to claim 1 and 2, it is characterized in that: described stablizer is natural and/or synthetic macromolecular compound, and it consists of one or more of multipolymer of hydroxypropylcellulose, ethyl cellulose, Polyvinylpyrolidone (PVP), polyvinyl acetate, polymethyl acrylic acid, polyvinyl alcohol, vinylbenzene and maleic anhydride; Preferred polyvinyl acetate: polymethyl acrylic acid is the mixture of 1:1.
4. according to each described preparation method of claim 1-3, it is characterized in that: described organic hydrocarbon solvent is selected from one or more in gasoline, kerosene, diesel oil or the white oil; Be preferably kerosene: diesel oil is the mixture of 1:1.
5. according to each described preparation method of claim 1-4, it is characterized in that: described initiator is selected from Potassium Persulphate, Sodium Persulfate, ammonium persulphate, benzoyl peroxide, lauroyl peroxide, cross two carbonic acid dicyclohexyl esters, cross the sad tert-butyl ester, cross sad tert-pentyl ester, cross in nonane diacid di tert butyl carbonate, the t-butyl peroxy-acetate one or more; Be preferably benzoyl peroxide.
6. according to each described preparation method of claim 1-5, it is characterized in that: 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 the 2'-azo two (2-methyl isopropyl cyanide).
7. according to each described preparation method of claim 1-6, it is characterized in that: in the described step 3, stirring velocity is 50～100r/min, and churning time is 5 minutes.
8. according to each described preparation method of claim 1-7, it is characterized in that: drying temperature is 90～120 ℃ in the described step 6, and be 2～3 hours time of drying.
9. according to each described preparation method of claim 1-8, it is characterized in that: comprise the steps:
(1) configuration sodium acrylate monomers solution: in material-compound tank, add 350 parts in vinylformic acid, 500 parts in water, the control temperature is 35 ℃, slowly dropping sodium is 350 parts;
(2) add 250 parts of sodium acrylate monomers solution respectively at the water jar; EDTA0.4 part; 3.5 parts of benzoyl peroxides; 8 parts of initiator azo-bis-iso-dimethyls; Stirring and dissolving is uniformly dispersed, and gets the monomer phase;
(3) be in 6 parts of adding reactors of stablizer of 1:1 with polyvinyl acetate and polymethyl acrylic acid mass ratio, add 550 parts of diesel oil simultaneously, put into then in the water-bath under the room temperature, stir with agitator, under liquid level, charge into nitrogen simultaneously;
(4) charge into 30 minutes nitrogen in the reactor after, add monomer below 35 ℃ at temperature of reaction kettle and stirred mutually 15 minutes, the speed of agitator is 180r/min, is adjusted to nitrogen tube on the liquid level and continues inflated with nitrogen;
(5) slowly temperature is raised to 70 ℃, reacted 2.5 hours, stop to fill nitrogen, begin distillation after being warmed up to 85 ℃, distillation time is 1.5 hours;
(6) after distillation is finished, product is sent into the drying machine drying, drying temperature is 100 ℃, and drying time is 2.5 hours, dry back packing and storing.
10. the prepared pearl sodium polyacrylate of each preparation method of claim 1-9.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105296437A (en) * | 2015-07-03 | 2016-02-03 | 上海诺百生物科技有限公司 | Method for concentrating slow viruses |
| CN105949361A (en) * | 2016-06-15 | 2016-09-21 | 湖州超能生化有限公司 | Preparation method of solid sodium polyacrylate |
| CN106699936A (en) * | 2016-12-01 | 2017-05-24 | 湖北硅金凝节能减排科技有限公司 | Preparation method of sodium polyacrylate with high molecular weight |
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| 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 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4647636A (en) * | 1984-09-19 | 1987-03-03 | Arakawa Kagaku Kogyo Kabushiki Kaisha | Process for preparing highly water-absorbent resin |
| JPH06287207A (en) * | 1993-02-03 | 1994-10-11 | Retsuku Tec Lab Kk | Production of soluble acrylic acid polymer granule |
| CN101215349A (en) * | 2007-12-26 | 2008-07-09 | 仲恺农业技术学院 | Preparation method of reversed phase suspension of sodium polyacrylate |
| CN101503559A (en) * | 2009-03-12 | 2009-08-12 | 中国科学院长春应用化学研究所 | Multifunctional emulsion for fruit bagging and preparation |
-
2013
- 2013-04-15 CN CN201310129918.1A patent/CN103242468B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4647636A (en) * | 1984-09-19 | 1987-03-03 | Arakawa Kagaku Kogyo Kabushiki Kaisha | Process for preparing highly water-absorbent resin |
| JPH06287207A (en) * | 1993-02-03 | 1994-10-11 | Retsuku Tec Lab Kk | Production of soluble acrylic acid polymer granule |
| CN101215349A (en) * | 2007-12-26 | 2008-07-09 | 仲恺农业技术学院 | Preparation method of reversed phase suspension of sodium polyacrylate |
| CN101503559A (en) * | 2009-03-12 | 2009-08-12 | 中国科学院长春应用化学研究所 | Multifunctional emulsion for fruit bagging and preparation |
Non-Patent Citations (5)
| Title |
|---|
| 联邦德国B.沃尔默特著、黄家贤等译: "《高分子化学基础》", 30 November 1986, article "助剂" * |
| 胡学贵主编: "《高分子化学及工艺学》", 31 May 1993, article "助剂", pages: 94 * |
| 胡建波等: "采用反相悬浮聚合法合成水溶性固体丙烯酸共聚物", 《棉纺织技术》, vol. 32, no. 9, 30 September 2004 (2004-09-30), pages 526 - 529 * |
| 邹胜林等: "反相悬浮法合成高分子量聚丙烯酸钠", 《化学反应工程与工艺》, vol. 18, no. 4, 31 December 2002 (2002-12-31), pages 294 - 298 * |
| 陈雪萍等: "水溶性高分子量聚丙烯酸钠的合成工艺", 《化工生产与技术》, vol. 11, no. 1, 31 December 2004 (2004-12-31), pages 37 - 39 * |
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