CN104086704A - Starch grafted acrylamide and preparation method and application thereof - Google Patents
Starch grafted acrylamide and preparation method and application thereof Download PDFInfo
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- CN104086704A CN104086704A CN201410265501.2A CN201410265501A CN104086704A CN 104086704 A CN104086704 A CN 104086704A CN 201410265501 A CN201410265501 A CN 201410265501A CN 104086704 A CN104086704 A CN 104086704A
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Abstract
The invention discloses starch grafted acrylamide and a preparation method and application thereof. The preparation method comprises the following steps: preparing waxy corn starch milk and adding an expansion inhibitor; adding alkali to adjust the starch milk to a certain pH value, adding a cationic reagent, and performing a cationic reaction at the temperature of 70-90 DEG C; taking acrylamide as a monomer, adding an initiating agent, performing a graft copolymerization reaction in a water phase of 40-80 DEG C, separating, drying and smashing to obtain the starch grafted acrylamide. By adding the prepared starch grafted acrylamide into the wet part of a papermaking machine in a certain mass ratio, the physical strength of produced paper can be enhanced.
Description
Technical field
The invention belongs to polymer fabricating technology field, be specifically related to a kind of starch graft acrylamide and preparation method thereof and application.
Background technology
Starch resource is abundant, is widely used in the industries such as food, papermaking, weaving, oil, has become a kind of important industrial raw materials, paper industry especially, and it is the first that its application percentage occupy.Starch is the natural polymers that a kind of amylopectin and amylose starch component are mixed naturally.Amylose starch has the character such as good film-forming properties, gelation, and the amylopectin function such as, freeze-thaw stability anti-aging because having, thickening, high-expansion and water-absorbent is widely used in food, wrapping material, the water-soluble and field such as Biodegradable films, medicine and building industry.
Waxy corn starch is that full branched structure is a kind of natural highly branched semi-rigid polymer macromole, the constitutional features of its molecular chain shows as and is pencil branched structure, and wherein main chain is formed by connecting by alpha-1, 4-glucosidic key, side chain is connected with main chain by alpha-1, 6-glucosidic key.Utilize this constitutional features, by Raolical polymerizable, can realize the copolymerization of its molecular chain avtive spot and water-soluble vinyl monomer, form the high degree of branching water-soluble graft polymers with property.
CN102875742A discloses the manufacture method that a kind of amylopectin is the high degree of branching acrylamide grafted copolymer of skeleton: amylopectin, water-soluble vinyl monomer and response type surfactant active carry out free radical grafting reaction, adds cross-linking monomer and linking agent and carries out modified-reaction and prepare the high degree of branching, lightly crosslinked water miscible graftomer.
The physical and chemical state of the < < starch that Li Mingda, Zhou Yongyuan in 2002 deliver is mentioned the easy gelatinization of amylopectin to affecting in > > literary composition of starch-grafted super absorbent resin water absorbing properties, and graft copolymerization is had to promoter action.
CN102617799A discloses a kind of preparation method of starch graft acrylamide paper strengthening agent, it is first starch to be oxidized, and then carry out positive ionization, after product is carried out to gelatinization, take acrylamide, cationic monomer carries out graft copolymerization as mixed grafting monomer again.In this process, reactions steps is too much, will affect the productive rate of the finished product; After positive ionization, also need cationic starch to carry out solvability and the stability in storage that the increase of gelatinization energy consumption and final product impurity too much can affect product.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is to provide a kind of preparation method of starch graft acrylamide, this preparation method's mild condition, and products obtained therefrom reinforced effects is good, applied widely, excellent storage stability.
The starch graft acrylamide that provides above-mentioned preparation method to obtain is provided.
A further object of the present invention is to provide the application of the starch graft acrylamide that above-mentioned preparation method obtains.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for starch graft acrylamide, comprises the following steps:
(1) waxy corn starch, expansion inhibitor and distilled water being mixed and made into massfraction is 10～50% starch suspension;
(2) add the pH value of the starch suspension that alkali lye obtains step (1) to be adjusted to 10～11, and the 15～30min that alkalizes; The cationic etherifying agent that is equivalent to waxy corn starch weight 6～8% is added in the starch suspension after alkalization, and is warming up to 70～90 ℃ of reaction 0.5～2h, obtain the starch paste of cationization;
(3) after the starch paste that step (2) obtained is cooling, add acrylamide monomer solution and initiator solution, under nitrogen protection, in 40～80 ℃ of waters, carry out graft copolymerization, the reaction times is 2～6h, obtains graft copolymer;
(4) graft copolymer step (3) being obtained to without precipitate, then obtains described starch graft acrylamide in 50～60 ℃ of vacuum-drying to constant weights with washing with acetone.
Preferably, the described expansion inhibitor of step (1) is 10～15% of waxy corn starch weight; Described expansion inhibitor is at least one in sodium-chlor or Repone K.
Preferably, the massfraction of the described alkali lye of step (2) is 10～20%; Alkali in described alkali lye is at least one in sodium hydroxide, potassium hydroxide or calcium hydroxide; Starch suspension alkalizes under 30 ℃ of conditions.
Preferably, the described cationic etherifying agent of step (2) is 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride or 2,3-epoxypropyltrimethylchloride chloride.
Preferably, the initiator in the described initiator solution of step (3) is a kind of in ceric ammonium nitrate, Potassium Persulphate, ammonium persulphate, Potassium Persulphate/S-WAT, Potassium Persulphate/sodium bisulfite, ammonium persulphate/S-WAT and ammonium persulphate/sodium bisulfite.
Preferably, the described initiator solution concentration of step (3) is 1～10mmol/L; Acrylamide monomer strength of solution is 0.5～1.5mol/L.
Preferably, Glacial acetic acid-ethylene glycol the mixed solvent that is 60:40 by volume ratio by the starch graft acrylamide of step (4) gained soaks 3～5 times, remove homopolymer, then with acetone, be washed till neutrality, again by product in 50～60 ℃ of vacuum-dryings to constant weight, after pulverizing, obtain starch graft acrylamide essence product.
The starch graft acrylamide that above-mentioned preparation method obtains.
The application of the starch graft acrylamide that above-mentioned preparation method obtains in improving paper strength.
Preferably, the concrete operation step of described application is: starch graft acrylamide is mixed with to the paper making intensifier solution that concentration is 0.001g/mL, then in 0.2～0.8% the ratio with respect to absolute dried paper pulp quality, paper making intensifier solution is added in paper machine wet pulp, to improve the intensity of paper.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) of the present inventionly by " single stage method ", prepare graft copolymer, process is simple, easy to operate, does not need the starch paste after cationization to carry out further gelatinization, has saved production time and cost.
(2) to take the waxy corn starch of full side chain be raw material in the present invention, by Raolical polymerizable, realize the copolymerization of its molecular chain avtive spot and water-soluble vinyl monomer, formation has the high degree of branching water soluble graft copolymerization thing of property, and it has good water conservation, thickening, temperature resistance, anti-shear performance; By graft copolymerization, the functional group of introducing, is conducive to the performance of reinforced effects, has also improved the package stability of product, and product can be stored with solution state, easy to use.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of acrylamide.
Fig. 2 is the infrared spectrogram of embodiment 1 starch graft acrylamide.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
A preparation method for starch graft acrylamide, comprises the following steps:
(1) waxy corn starch, expansion inhibitor and distilled water being mixed and made into massfraction is 10% starch suspension; Described expansion inhibitor is Repone K, and its addition is 15% of waxy corn starch weight;
(2) add the pH value of the starch suspension that alkali lye obtains step (1) to be adjusted to 11, and the 30min that alkalizes under 30 ℃ of conditions; The cationic etherifying agent that is equivalent to waxy corn starch weight 8% is added in the starch suspension after alkalization, and is warming up to 70 ℃ of reaction 1h, obtain the starch paste of cationization;
The massfraction of described alkali lye is 20%, and the alkali in described alkali lye is sodium hydroxide; Described cationic etherifying agent is 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride;
(3) after the starch paste that step (2) obtained is cooling, add acrylamide monomer solution and ceric ammonium nitrate solution, pass into nitrogen protection, in 50 ℃ of waters, carry out graft copolymerization, the reaction times is 2h, obtains graft copolymer; The acrylamide monomer strength of solution adding is 0.5mol/L, and the ceric ammonium nitrate solution concentration adding is 2mmol/L;
(4) graft copolymer step (3) being obtained, is then dried to constant weight and obtains the thick product of starch graft acrylamide to without precipitate with washing with acetone in 50 ℃ of vacuum drying ovens;
(5) Glacial acetic acid-ethylene glycol mixed solvent that is 60:40 by the thick product of starch graft acrylamide of step (4) gained by volume ratio soaks 3 times, remove homopolymer, then with acetone, be washed till neutrality, again product is dried to constant weight in 50 ℃ of vacuum drying ovens, after drying and crushing, obtains starch graft acrylamide multipolymer essence product.After testing, the finished product productive rate is 90%.
The starch graft acrylamide multipolymer of acrylamide monomer and the last gained of the present embodiment is done to infrared detection, and detected result respectively as depicted in figs. 1 and 2.In Fig. 2 at 3500cm
-1place has the characteristic peak of glucose ring to occur, although obvious absorption peak has also appearred in this scope in Fig. 1, is not so good as positively charged ion waxy corn starch graft acrylamide peak area herein large; And in Fig. 2, can obtain, at 1650～1690cm
-1between absorption peak obvious especially, this shows on starch graft acrylamide is amide group with C=O group, there is graft reaction in this explanation acrylamide and cationic starch.Cationic starch graft acrylamide is subject to the impact of acrylamide chain in molecule, and variation has also occurred in fingerprint region.
The above-mentioned starch graft acrylamide multipolymer preparing is applied to the toughener of Corrugating Base Paper, to improve paper strength, concrete operation step is: starch graft acrylamide multipolymer is mixed with to the paper making intensifier solution that concentration is 0.001g/mL, then in 0.4% the ratio with respect to absolute dried paper pulp quality, paper making intensifier solution is added in paper machine wet pulp, to improve the intensity of paper, can regulate its concentration and potential of hydrogen according to practical situation.
With 80gm
-2copy paper on standard sheet forming apparatus, then presses the character that national standard method is measured page.Tensile strength, pop strength, tear strength are measured according to GB/T453-2002, GB/T454-2002, GB/T455-2002 respectively.Corrugation paper after the enhancing finally obtaining is after testing compared with Corrugating Base Paper, and burst index amplification can reach 20%, and tear strength amplification can reach 25%, tensile strength amplification can reach 28%.
Embodiment 2
A preparation method for starch graft acrylamide, comprises the following steps:
(1) waxy corn starch, expansion inhibitor and distilled water being mixed and made into massfraction is 10% starch suspension; Add expansion inhibitor sodium-chlor, its addition is 10% of waxy corn starch weight;
(2) add the pH value of the starch suspension that alkali lye obtains step (1) to be adjusted to 11, and the 15min that alkalizes under 30 ℃ of conditions; The cationic etherifying agent that is equivalent to waxy corn starch weight 6% is added in the starch suspension after alkalization, and is warming up to 90 ℃ of reaction 1h, obtain the starch paste of cationization;
The massfraction of described alkali lye is 20%, and the alkali in described alkali lye is sodium hydroxide; Described cationic etherifying agent is 2,3-epoxypropyltrimethylchloride chloride;
(3) after the starch paste that step (2) obtained is cooling, add acrylamide monomer solution and potassium persulfate solution, pass into nitrogen protection, in 40 ℃ of waters, carry out graft copolymerization, the reaction times is 2h, obtains graft copolymer; The acrylamide monomer strength of solution adding is 1mol/L, and the potassium persulfate solution concentration adding is 4mmol/L;
(4) graft copolymer step (3) being obtained, is then dried to constant weight and obtains the thick product of starch graft acrylamide to without precipitate with washing with acetone in 50 ℃ of vacuum drying ovens;
(5) Glacial acetic acid-ethylene glycol mixed solvent that is 60:40 by the thick product of starch graft acrylamide of step (4) gained by volume ratio soaks 5 times, remove homopolymer, then with acetone, be washed till neutrality, again product is dried to constant weight in 60 ℃ of vacuum drying ovens, after drying and crushing, obtains starch graft acrylamide essence product.After testing, the finished product productive rate is 93%.
The above-mentioned starch graft acrylamide multipolymer preparing is applied to the toughener of newsprint, to improve paper strength, concrete operation step is: starch graft acrylamide multipolymer is mixed with to the paper making intensifier solution that concentration is 0.001g/mL, then in 0.4% the ratio with respect to absolute dried paper pulp quality, paper making intensifier solution is added in paper machine wet pulp, to improve the intensity of paper, can regulate its concentration and potential of hydrogen according to practical situation.According to the detection method of embodiment 1, the paper detecting after the enhancing finally obtain is compared with original news paper, and burst index amplification can reach 20%, and tear strength amplification can reach 22%, tensile strength amplification can reach 27%.
Embodiment 3
A preparation method for starch graft acrylamide, comprises the following steps:
(1) waxy corn starch, expansion inhibitor and distilled water being mixed and made into massfraction is 50% starch suspension; Described expansion inhibitor is Repone K, and its addition is 15% of waxy corn starch weight;
(2) add the pH value of the starch suspension that alkali lye obtains step (1) to be adjusted to 10, and the 20min that alkalizes under 30 ℃ of conditions; The cationic etherifying agent that is equivalent to waxy corn starch weight 8% is added in the starch suspension after alkalization, and is warming up to 70 ℃ of reaction 0.5h, obtain the starch paste of cationization;
The massfraction of described alkali lye is 10%, and the alkali in described alkali lye is potassium hydroxide; Described cationic etherifying agent is 2,3-epoxypropyltrimethylchloride chloride;
(3) after the starch paste that step (2) obtained is cooling, add acrylamide monomer solution and ammonium persulfate solution, pass into nitrogen protection, in 40 ℃ of waters, carry out graft copolymerization, the reaction times is 6h, obtains graft copolymer; The acrylamide monomer strength of solution adding is 1mol/L, and the ammonium persulfate solution concentration adding is 6mmol/L;
(4) graft copolymer step (3) being obtained, is then dried to constant weight and obtains the thick product of starch graft acrylamide to without precipitate with washing with acetone in 60 ℃ of vacuum drying ovens;
(5) Glacial acetic acid-ethylene glycol mixed solvent that is 60:40 by the thick product of starch graft acrylamide of step (4) gained by volume ratio soaks 3 times, remove homopolymer, then with acetone, be washed till neutrality, again product is dried to constant weight in 50 ℃ of vacuum drying ovens, after drying and crushing, obtains starch graft acrylamide essence product.After testing, the finished product productive rate is 91%.
The above-mentioned starch graft acrylamide multipolymer preparing is applied to the toughener of cultural paper, to improve paper strength, concrete operation step is: starch graft acrylamide multipolymer is mixed with to the paper making intensifier solution that concentration is 0.001g/mL, then in 0.8% the ratio with respect to absolute dried paper pulp quality, paper making intensifier solution is added in paper machine wet pulp, to improve the intensity of paper, can regulate its concentration and potential of hydrogen according to practical situation.According to the detection method of embodiment 1, the cultural paper detecting after the enhancing finally obtain is compared with original cultural paper, and burst index amplification can reach 23%, and tear strength amplification can reach 30%, tensile strength amplification can reach 30%.
Embodiment 4
A preparation method for starch graft acrylamide, comprises the following steps:
(1) waxy corn starch, expansion inhibitor and distilled water being mixed and made into massfraction is 30% starch suspension; Described expansion inhibitor is sodium-chlor, and its addition is 15% of waxy corn starch weight;
(2) add the pH value of the starch suspension that alkali lye obtains step (1) to be adjusted to 11, and the 30min that alkalizes under 30 ℃ of conditions; The cationic etherifying agent that is equivalent to waxy corn starch weight 8% is added in the starch suspension after alkalization, and is warming up to 90 ℃ of reaction 0.5h, obtain the starch paste of cationization;
The massfraction of described alkali lye is 10%, and the alkali in described alkali lye is sodium hydroxide; Described cationic etherifying agent is 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride;
(3) after the starch paste that step (2) obtained is cooling, add acrylamide monomer solution and initiator potassium persulfate/sodium sulfite solution, pass into nitrogen protection, in 80 ℃ of waters, carry out graft copolymerization, reaction times is 6h, obtains graft copolymer; The acrylamide monomer strength of solution adding is 1.5mol/L, and the Potassium Persulphate/sodium sulfite solution concentration adding is 10mmol/L;
(4) graft copolymer step (3) being obtained, is then dried to constant weight and obtains the thick product of starch graft acrylamide to without precipitate with washing with acetone in 60 ℃ of vacuum drying ovens;
(5) Glacial acetic acid-ethylene glycol mixed solvent that is 60:40 by the thick product of starch graft acrylamide of step (4) gained by volume ratio soaks 5 times, remove homopolymer, then with acetone, be washed till neutrality, again product is dried to constant weight in 60 ℃ of vacuum drying ovens, after drying and crushing, obtains starch graft acrylamide essence product.After testing, the finished product productive rate is 92%.
The above-mentioned starch graft acrylamide multipolymer preparing is applied to the toughener of waste and old boxboard, to improve paper strength, concrete operation step is: starch graft acrylamide multipolymer is mixed with to the paper making intensifier solution that concentration is 0.001g/mL, then in 0.4% the ratio with respect to absolute dried paper pulp quality, paper making intensifier solution is added in paper machine wet pulp, to improve the intensity of paper, can regulate its concentration and potential of hydrogen according to practical situation.According to the detection method of embodiment 1, the waste and old boxboard detecting after the enhancing finally obtain is compared with original waste and old boxboard, and burst index amplification can reach 22%, and tear strength amplification can reach 27%, tensile strength amplification can reach 26%.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. a preparation method for starch graft acrylamide, is characterized in that, comprises the following steps:
(1) waxy corn starch, expansion inhibitor and distilled water being mixed and made into massfraction is 10～50% starch suspension;
(2) add the pH value of the starch suspension that alkali lye obtains step (1) to be adjusted to 10～11, and the 15～30min that alkalizes; The cationic etherifying agent that is equivalent to waxy corn starch weight 6～8% is added in the starch suspension after alkalization, and is warming up to 70～90 ℃ of reaction 0.5～2h, obtain the starch paste of cationization;
(3) after the starch paste that step (2) obtained is cooling, add acrylamide monomer solution and initiator solution, under nitrogen protection, in 40～80 ℃ of waters, carry out graft copolymerization, the reaction times is 2～6h, obtains graft copolymer;
(4) graft copolymer step (3) being obtained to without precipitate, then obtains described starch graft acrylamide in 50～60 ℃ of vacuum-drying to constant weights with washing with acetone.
2. preparation method according to claim 1, is characterized in that, the described expansion inhibitor of step (1) is 10～15% of waxy corn starch weight; Described expansion inhibitor is at least one in sodium-chlor or Repone K.
3. preparation method according to claim 1, is characterized in that, the massfraction of the described alkali lye of step (2) is 10～20%; Alkali in described alkali lye is at least one in sodium hydroxide, potassium hydroxide or calcium hydroxide; Starch suspension alkalizes under 30 ℃ of conditions.
4. preparation method according to claim 1, is characterized in that, the described cationic etherifying agent of step (2) is 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride or 2,3-epoxypropyltrimethylchloride chloride.
5. preparation method according to claim 1, it is characterized in that, the initiator in the described initiator solution of step (3) is a kind of in ceric ammonium nitrate, Potassium Persulphate, ammonium persulphate, Potassium Persulphate/S-WAT, Potassium Persulphate/sodium bisulfite, ammonium persulphate/S-WAT and ammonium persulphate/sodium bisulfite.
6. preparation method according to claim 1, is characterized in that, the described initiator solution concentration of step (3) is 1～10mmol/L; Acrylamide monomer strength of solution is 0.5～1.5mol/L.
7. preparation method according to claim 1, it is characterized in that, Glacial acetic acid-ethylene glycol the mixed solvent that is 60:40 by volume ratio by the starch graft acrylamide of step (4) gained soaks 3～5 times, then with acetone, be washed till neutrality, again by product in 50～60 ℃ of vacuum-dryings to constant weight, after pulverizing, obtain starch graft acrylamide essence product.
8. the starch graft acrylamide that described in claim 1～7 any one, preparation method obtains.
9. the application of the starch graft acrylamide that described in claim 1～7 any one, preparation method obtains in improving paper strength.
10. application according to claim 9, it is characterized in that, the concrete operation step of described application is: starch graft acrylamide is mixed with to the paper making intensifier solution that concentration is 0.001g/mL, then in 0.2～0.8% the ratio with respect to absolute dried paper pulp quality, paper making intensifier solution is added in paper machine wet pulp.
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| CN104356301A (en) * | 2014-11-06 | 2015-02-18 | 黑龙江科技大学 | Preparation method of polymeric flocculant |
| CN106007119A (en) * | 2016-06-02 | 2016-10-12 | 陈昌 | Method for treating city sewage |
| CN106543365A (en) * | 2015-09-18 | 2017-03-29 | 上海东升新材料有限公司 | A kind of method for preparing acrylic amide modified tapioca |
| CN109336239A (en) * | 2018-08-13 | 2019-02-15 | 华电电力科学研究院有限公司 | A kind of preparation method of high solubility starch graft modification cationic flocculant |
| CN109485794A (en) * | 2018-12-25 | 2019-03-19 | 昆山裕锦环保包装有限公司 | A kind of preparation method and applications of starch graft acrylamide |
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| CN104356301A (en) * | 2014-11-06 | 2015-02-18 | 黑龙江科技大学 | Preparation method of polymeric flocculant |
| CN104356301B (en) * | 2014-11-06 | 2017-09-15 | 黑龙江科技大学 | A kind of high polymer coagulant preparation method |
| CN106543365A (en) * | 2015-09-18 | 2017-03-29 | 上海东升新材料有限公司 | A kind of method for preparing acrylic amide modified tapioca |
| CN106007119A (en) * | 2016-06-02 | 2016-10-12 | 陈昌 | Method for treating city sewage |
| CN109336239A (en) * | 2018-08-13 | 2019-02-15 | 华电电力科学研究院有限公司 | A kind of preparation method of high solubility starch graft modification cationic flocculant |
| CN109535319A (en) * | 2018-11-07 | 2019-03-29 | 济宁明升新材料有限公司 | A kind of environmentally friendly drying strengthening agent and preparation method thereof |
| CN109653025A (en) * | 2018-12-12 | 2019-04-19 | 济宁明升新材料有限公司 | A kind of preparation method of natural polysaccharide and its derivative modified wet strengthening agents for papermaking |
| CN109679026A (en) * | 2018-12-12 | 2019-04-26 | 济宁明升新材料有限公司 | A kind of emulsion-type modified starch drying strengthening agent and preparation method thereof |
| CN109485794A (en) * | 2018-12-25 | 2019-03-19 | 昆山裕锦环保包装有限公司 | A kind of preparation method and applications of starch graft acrylamide |
| CN109749012A (en) * | 2019-01-24 | 2019-05-14 | 湖北中之天科技股份有限公司 | A kind of production method of the environment-friendly type without chlorine polyacrylamide wet strength agent and the application in papermaking |
| CN109989292A (en) * | 2019-03-01 | 2019-07-09 | 徐扣华 | A kind of preparation method of starch base sticking agent |
| CN114989355A (en) * | 2022-05-09 | 2022-09-02 | 华南理工大学 | Hydroxypropyl grafted acrylamide starch for dry-mixed masonry mortar and preparation |
| CN114989355B (en) * | 2022-05-09 | 2023-08-22 | 华南理工大学 | Hydroxypropyl grafted acrylamide starch for dry-mixed masonry mortar and preparation method thereof |
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