CN103045702A - Method for producing modified starch size through bio-enzyme - Google Patents
Method for producing modified starch size through bio-enzyme Download PDFInfo
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- CN103045702A CN103045702A CN2012105297142A CN201210529714A CN103045702A CN 103045702 A CN103045702 A CN 103045702A CN 2012105297142 A CN2012105297142 A CN 2012105297142A CN 201210529714 A CN201210529714 A CN 201210529714A CN 103045702 A CN103045702 A CN 103045702A
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Abstract
The invention discloses a method for producing grafted starch size through bio-enzyme. The method adopts ultronic assistant debranching enzyme to pretreat original starch, the macromolecular structure and molecular weight of the starch are adjusted, and the masses of different types of enzymes are stabilized; and a mixed initiating system which consists of horse radish peroxidase, hydrogen peroxide and beta-diketone is utilized to initiate the graft copolymerization of the starch and acrylic acid monomers, and a polyacrylic acid branch is connected to a starch macromolecule. According to the method, the bio-enzyme is adopted to modify the starch, the reaction conditions are moderate, and the activity is controllable; the horse radish peroxidase initiates the polymerization reaction, so that low-temperature branching polymerization can be effectively realized, and the temperature of an initiation process is controlled stably; and the polymerization product has low viscosity and is easy to separate.
Description
Technical field
The present invention relates to the jean yarn starching preparation of modified starch spinning sizing agent, particularly a kind of production method for preparing grafting starch by biological enzyme.
Background technology
Most denims are slightly to prop up high density fabric, and the fabric compactness coefficient is higher, and the cloth cover requirement is smooth, lines is clear, for reaching this effect, will adopt hightension, thwack latitude technique when weaving, and many shuttleless weaving machines fast in speed, that tension force is large are weaved.Most of denims all adopt rotor spun yarn production, and its brute force is than the low 10-20% of ring spun yarn; And denim adopts the operational path of sizing after the first dyeing, and warp thread is subject to larger damage than nature fabric before sizing, need remedy through sizing, weaves environment to adapt to, so warp sizing is one of denim critical process of producing.Make smooth, wear-resisting, the pliable and tough serous coat with some strength of the surface-coated one deck of warp thread by starching, make simultaneously the part slurry infiltrate the inside of yarn, increase interfibrous adhesive power, improve tensile strength, frictional strength and the subsides volt filoplume of yarn, and then reach the purpose that reduction is weaved end breakage rate, enhanced productivity, improves quality product.
It is with a long history that starch is used for warp sizing, ative starch has preferably adhesivity to hydrophilic natural fiber, has certain film forming ability, though but the intensity of gained serous coat is high after the starch size starching, elongation at break is little, and Young's modulus is large, work of rupture is very little, a little less than the yield strength, toughness is also poor, and the various sizing agents of often needs interpolation are remedied or starch is carried out denaturing treatment.The modified starch that mostly is that is widely used at present the textile warp starching, three generation products is gone through in the development of modified starch, first on behalf of starch-splitting, it is to cut off the glycosidic bond on the starch polymer, reduce the polymerization degree and viscosity, increasing working concentration and water dispersible is main purpose, and product comprises acidified starch, Sumstar 190, enzymolysis starch etc.Second on behalf of starch derivative, introduces some chemical group in starch molecule, take the water dispersible, gel resistance, serous coat characteristic and the clinging power that improve slurries as main purpose, such as etherification starch, esterification starch and cationic starch etc.Graft starch is third generation product, graft starch normally adopts vinyl monomer to cause at the starch polymer main chain by radical and forms the synthetic macromolecule side chain with certain polymerization degree, this product has the dual property of native starch and synthetic macromolecule, because grafted branches has certain polymerization degree, reduce the regularity of starch polymer chain packing, caused intermolecular accumulation loose.In addition, grafted branches is generally formed by the lower flexible monomer polymerization of second-order transition temperature, so that the second-order transition temperature of grafting modified starch reduces, flexibility increases, and therefore starch-grafted sex change can improve the snappiness of serous coat, greatly improves the film-forming properties of starch size.Graft starch itself has two phase separation structures, has greatly improved the mechanical property of starch.Because these potential advantages add good biodegradability, graft starch has caused the very big concern of textile limit in recent years.Graft starch is not only possessed the high-performance of starch size on warp sizing, also have the tack good to hydrophobic fibre that other modified starch sizes do not have.
The preparation of starch graft copolymer is to carry out in the mode of radical polymerization mostly, and the key of development graft starch is to seek a kind of effective initiator or initiation method, produces active group at starch molecular chain.Usually the method for living radical has chemical method, Physical and biological process.The physics initiating method is to utilize radioactive element
60Gamma-radiation irradiation and the electron beam irradiation starch of Co produce free radical, Inducing Graft Polymerization, i.e. high-energy radiation initiation grafting.The physics initiating method reacts wayward because quantity of radiant energy is high, can affect the bulk properties of starch; And it is higher that irradiation causes the investment of equipment, and ray has than major injury operator's health and is difficult to use.It then is the most frequently used method that chemical method cause to produce free radical, this wherein most popular chemical initiating method be starch and the reaction of high price cerium ion, but the high price cerium ion is expensive at present, output is limited and its application is restricted.Also there is the difficult problem of grafts and homopolymer separating-purifying simultaneously in the chemistry initiating method.Biological initiation mainly is the effect initiated polymerization by enzyme, compare with traditional chemical initiated polymerization, have reaction conditions gentleness, active controlled, good product selectivity, the advantage such as efficient, green, for starch-based graft copolymer further develop and use significant.
Summary of the invention
The present invention is directed to chemical method and Physical and produce the shortcoming that exists in the graft starch process, a kind of method of utilizing biological enzyme production to be fit to the graft starch of jean yarn starching is provided, adopt debranching factor that ative starch is carried out pre-treatment, the mixed system that utilizes subsequently horseradish peroxidase, hydrogen peroxide and beta-diketon to form causes starch and acrylic acid graft copolymerization generates grafting starch.The biological enzyme initiated polymerization can effectively be realized under the cold condition initiation grafting reaction, and the control of elicitation procedure temperature steadily causes effectively, and graft starch product separation process is simple.
The present invention is expensive for solving graft starch preparation process initiator, efficiency of initiation is lower, the product grafting efficiency hangs down shortcomings such as reaching graft starch product separation difficulty, propose to adopt debranching factor that ative starch is carried out pre-treatment, reduce the branched structure in the ative starch, adjust the structure of starch polymer, make it to form the relatively low amylose starch of molecular weight.The mixed initiating system that utilizes subsequently horseradish peroxidase, hydrogen peroxide and beta-diketon to form causes the graft copolymerization of starch and acrylic monomer, the grafting starch of access polyacrylic side chain in starch polymer, this grafting starch can directly substitute tradition and contain the combined slurry of PVA for the starching of jean yarn.
Ative starch mainly is comprised of amylose starch and amylopectin.Amylose molecule connects chaining by anhydroglucose with α-Isosorbide-5-Nitrae-glycosidic bond, and with α-Isosorbide-5-Nitrae-glycosidic bond or α-1, the 6-glycosidic bond connects chaining to amylopectin by anhydroglucose, and its side chain tie point is α-1, the 6-glycosidic bond, and the molecular weight ratio amylose starch of amylopectin is higher.The content of amylopectin is higher than amylose starch far away in most ative starchs, and the starch molecule amount is very large, and its quality is subjected to various factors and unstable, therefore at first ative starch is adopted the debranching factor pre-treatment.The α-1 of debranching factor in can the selective hydrolysis branched structure, the 6-glycosidic link, thus cut the whole side shoot of amylopectin, make amylopectin become amylose starch, regulate the molecular weight of starch molecule, improve starch use procedure rheological properties, improve Size-Film Forming Properties etc.
It is the novel enzymatic initiator system that utilizes horseradish peroxidase (HRP), hydrogen peroxide and beta-diketon to consist of that so-called biological enzyme causes the copolymerized grafting reaction.Horseradish peroxidase is a kind of Ferri-hemoglobin that contains, and by the peptide chain that 308 amino acid form, prothetic group is protoheme, relative molecular mass is about 44000, the catalytic mechanism of HRP is a peroxidation working cycle, on the ferro element and porphyrin ring of HRP avtive spot in the Ferri-hemoglobin molecule, and H
2O
2Heterolytic fission occurs in molecule under the HRP molecularity, two portions of heterolytic fission and HRP generate the transition state complex compound, then in enzyme active sites generation bielectron oxidising process, generate a π-radical cation HRP-I, the HRP-I is the catalysis intermediate of a high oxidation state, comprises one and contains oxygen Fe (IV) center and a positively charged porphyrin.The hydrogen atom that the HRP-I can be captured in the beta-diketon molecular structure obtains compound H RP-II and the elementary free radical of beta-diketon.The HRP-II equally also is the catalysis intermediate of high oxidation state, redox-potential approaches+1V, it can continue to capture the hydrogen atom in the beta-diketon molecular structure and then be returned to initial state by the one-electron oxidation reduction reaction, and the beta-diketon molecule is oxidized into the elementary free radical of beta-diketon, such enzymatic circulation just can produce two initial free radicals, shown in equation 1-4, the porphyrin ring in the equation with
Replace.
Starch polymer in two elementary free radicals of beta-diketon and the solution reacts, and can capture the hydrogen atom of hydroxyl on starch polymer C2 or the C3 atom, produces the starch polymer free radical in amylose molecule, shown in equation 5.
Acrylic monomer generation transfer reaction in starch polymer free radical and the system, in starch polymer C2 or C3 atom access acrylic acid or the like grafted branches, shown in equation 6, the R in the formula is sodium, alkane group etc.
By the enzymatic reaction in two steps, the generation main chain is starch molecule, and side chain is the graft starch of acrylic polymers structure, the reaction process mild condition, and operation control is steadily.
Implementing technical scheme of the present invention comprises the steps:
1) common starch is added the starch milk of the starch-containing 30-40% of deionized water furnishing, normal temperature is transferred in the processor for ultrasonic wave, heat up as 40-50 ℃, open supersound process 15-25 min, be 4-6 with the vinegar acid for adjusting pH value, add an amount of debranching factor, behind 40-55 ℃ of reaction 4-10 h, be warming up to 80 ℃ of reaction 30 min and make the debranching factor inactivation.
2) add a small amount of sodium bicarbonate in the starch milk that makes to step 1), the pH value of conditioned reaction system is 8-9, leads to nitrogen 15-30 min, removes the dissolved oxygen in the system.
3) an amount of beta-diketon and HRP solution are mixed to join in the starch milk, after stirring, drip simultaneously mass concentration in the system and be 30% H
2O
2With the mixing solutions of acrylic monomer, the temperature that keeps system is 35-45 ℃ of reaction 2-5 h.After reaction finishes, filter washing, the graft starch that obtains loosening, graft starch is dry, obtain grafting starch after pulverizing, sieving.
Above-mentioned starch comprises W-Gum, yam starch, wheat starch, tapioca (flour), Starch rice, any one in the sweet potato starch.
Above-mentioned used debranching factor is a kind of starch carbohydrase, and the mixture of one or both enzymes in Starch debranching enzyme, isoamylase, the limit dextrinase is arranged.The consumption of debranching factor is the 0.1-0.5% of dry starch consumption.
Above-mentioned used HRP is the general name of a class isozyme, wherein take Fluorescent study as main active ingredient.HRP, H
2O
2(30%) jointly consist of the graft copolymerization initiator system with beta-diketon, its mass ratio is 1:200:100.The consumption of HRP is the 0.01-0.1% of dry starch consumption (quality).
The above-mentioned used acrylic monomer that contains comprises one or more monomer mixtures in vinylformic acid, vinyl cyanide, methyl acrylate, ethyl propenoate, the butyl acrylate.The monomer consumption is the 10-25% of dry starch consumption.The mix monomer ratio changes, and can produce and be applicable to the needed serial slurry of different yarns kind.
The grafting starch that the present invention produces is compared with traditional slurry, and its advantage is as follows:
1) the present invention adopts the auxiliary biological enzyme of ultrasonic wave that ative starch is carried out pre-treatment, and the treatment temp of starch milk system is lower, the system viscosity acute variation of having avoided starch pasting to cause, and the method operating procedure is simple, energy consumption is low.
2) the present invention adopts horseradish peroxidase, hydrogen peroxide, beta-diketon jointly to consist of initiator system initiation starch polymer and forms free radical, and initiation conditions is gentle, occurs when having avoided traditional starch polymerization and gelatinization.Polymerisate viscosity of the present invention is lower, and product separation is comparatively easy, has solved the difficult problem of present modified starch aftertreatment.
3) grafting starch produced of the present invention is used in the starching of jean yarn, can substitute traditional combined slurry with single slurry, thoroughly solves complexity before the traditional starching process of sizing mixing, and has shortened starching process period.
4) graft starch production method suitability of the present invention is wider, different polymerization single polymerization monomers and dissimilar starch-grafted polymerization, can produce applicable textile, wash/the starching requirement of cotton blending yarn.
Embodiment
Below in conjunction with formulation examples the present invention is specifically described.
Embodiment 1
Take by weighing in the 8.5 g vinylformic acid, the NaOH solution of adding 20% is neutralized to the pH to 5-7 of solution, preparing propone acid sodium solution.Be that 40% acrylic acid solution mixes as the grafted monomer mixture with the sodium acrylate solution that makes with 160 g concentration.The starch milk that potato common starch 500 g is added deionized water furnishing starch-containing 30%, normal temperature is transferred in the processor for ultrasonic wave, be warming up to 40 ℃, open supersound process 20 min, be 4-6 with the vinegar acid for adjusting pH value, add debranching factor 1 g, stir, behind 40 ℃ of insulation reaction 5 h, be warming up to 80 ℃ of reaction 30 min and make the debranching factor inactivation.Add sodium bicarbonate aqueous solution in the starch milk that makes, the pH value of conditioned reaction system is 8-9, and logical nitrogen 20 min remove the dissolved oxygen in the solution.After the HRP that takes by weighing 25 g methyl ethyl diketones and 250 mL concentration and be 1 mg/L mixes, join in the starch milk that has prepared, drip simultaneously mass concentration in the system and be 30% H
2O
2With the acrylic monomer mixing solutions, the temperature that keeps system is 45 ℃ of reaction 2 h, after reaction finishes, filters washing, the graft starch that obtains loosening.Graft starch is dry, obtain grafting starch after pulverizing, sieving.
The percentage of grafting of this grafting starch is 12.1%, and monomer-grafted efficient is 74.5%.This stock quality concentration is 6%, and when gelatinization point was 90 ℃, the viscosity of dextrin was 14.4 cp, viscosity fluctuation rate＜10%, and slurry is 68.7 N to the adhesive power of purified cotton yarns, elongation at break is 8.3%.
Embodiment 2
Take by weighing 62 g vinylformic acid and 13 g butyl acrylates mix, as the graft copolymerization monomer.The starch milk that conventional corn starch 500 g is added deionized water furnishing starch-containing 30%, normal temperature is transferred in the processor for ultrasonic wave, be warming up to 40 ℃, open supersound process 20 min, be 4-6 with the vinegar acid for adjusting pH value, add debranching factor 1 g, stir, behind 40 ℃ of insulation reaction 5 h, be warming up to 80 ℃ of reaction 30 min and make the debranching factor inactivation.Add sodium bicarbonate aqueous solution in the starch milk that makes, the pH value of conditioned reaction system is 8-9, and logical nitrogen 20 min remove the dissolved oxygen in the solution.After the HRP that takes by weighing 25 g methyl ethyl diketones and 250 mL concentration and be 1 mg/L mixes, join in the starch milk that has prepared, drip simultaneously mass concentration in the system and be 30% H
2O
2With the acrylic monomer mixing solutions, the temperature that keeps system is 45 ℃ of reaction 2h.After reaction finishes, filter washing, the graft starch that obtains loosening.Graft starch is dry, obtain grafting starch after pulverizing, sieving.
The percentage of grafting of this grafting starch is 10.8%, and monomer-grafted efficient is 69.4%.This stock quality concentration is 6%, and when gelatinization point was 90 ℃, the viscosity of dextrin was 16.8 cp, viscosity fluctuation rate＜12%, and slurry is 74.5N to the adhesive power of purified cotton yarns, elongation at break is 10.6%.
Embodiment 3
Take by weighing 18 g vinylformic acid and 12 g ethyl propenoates mix, as the graft copolymerization monomer.The starch milk that conventional corn starch 200 g is added deionized water furnishing starch-containing 30%, normal temperature is transferred in the processor for ultrasonic wave, be warming up to 40 ℃, open supersound process 15 min, be 4-6 with the vinegar acid for adjusting pH value, add debranching factor 0.4 g, stir, behind 40 ℃ of insulation reaction 3 h, be warming up to 80 ℃ of reaction 20 min and make the debranching factor inactivation.Add sodium bicarbonate aqueous solution in the starch milk that makes, the pH value of conditioned reaction system is 8-9, and logical nitrogen 15 min remove the dissolved oxygen in the solution.After the HRP that takes by weighing 1 g methyl ethyl diketone and 100 mL concentration and be 1 mg/L mixes, join in the starch milk that has prepared, drip simultaneously mass concentration in the system and be 30% H
2O
2With the acrylic monomer mixing solutions, the temperature that keeps system is 45 ℃ of reaction 2 h.After reaction finishes, filter washing, the graft starch that obtains loosening.Graft starch is dry, obtain grafting starch after pulverizing, sieving.
The percentage of grafting of this grafting starch is 14.5%, and monomer-grafted efficient is 73.4%.This stock quality concentration is 6%, and when gelatinization point was 90 ℃, the viscosity of dextrin was 17.3 cp, viscosity fluctuation rate＜12%, and slurry is 84.2N to the adhesive power of purified cotton yarns, elongation at break is 9.6%.
Although the present invention illustrates and describes with reference to embodiment, will be understood by those skilled in the art that, in the situation that does not break away from the spirit and scope of the present invention that the appended claims limit, can carry out the various changes of form and details.
Claims (5)
1. the manufacture method of a modified starch size, it comprises the steps:
1) common starch is added the starch milk of the starch-containing 30-40% of deionized water furnishing, at 40-50 ℃ of supersound process 15-25 min, be 4-6 with the vinegar acid for adjusting pH value, add an amount of debranching factor, behind 40-55 ℃ of reaction 4-10 h, be warming up to 80 ℃ of reaction 30 min and make the debranching factor inactivation.
2) add a small amount of sodium bicarbonate in the starch milk that makes, the pH value of conditioned reaction system is 8-9, and logical nitrogen 15-30 min removes the dissolved oxygen in the system.
3) an amount of beta-diketon and horseradish peroxidase solution are mixed to join in the starch milk, after stirring, drip simultaneously mass concentration in the system and be 30% H
2O
2With the acrylic acid or the like mixed monomer solution, the temperature that keeps system is 35-45 ℃ of reaction 2-5 h, after reaction finishes, filters washing, the graft starch that obtains loosening.
2. the manufacture method of modified starch size according to claim 1, it is characterized in that: described common starch is any one in W-Gum, yam starch, wheat starch, tapioca (flour), Starch rice, the sweet potato starch.
3. the manufacture method of modified starch size according to claim 1, it is characterized in that: used debranching factor is the mixture of one or both enzymes in Starch debranching enzyme, isoamylase, the limit dextrinase, and the consumption of described debranching factor is the 0.1-0.5% of dry starch consumption.
4. the manufacture method of modified starch size according to claim 1 is characterized in that: used horseradish peroxidase, H
2O
2(30%) mass ratio with beta-diketon is 1:200:100, and the consumption of horseradish peroxidase is the 0.01-0.1% of dry starch consumption.
5. the manufacture method of modified starch size according to claim 1, it is characterized in that: used acrylic monomer is one or more monomer mixtures in vinylformic acid, vinyl cyanide, methyl acrylate, ethyl propenoate, the butyl acrylate.
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| CN103436572A (en) * | 2013-08-14 | 2013-12-11 | 江南大学 | Preparation method of tubular starch derivative |
| CN104418971A (en) * | 2013-09-09 | 2015-03-18 | 同济大学 | Glucose oxidase mediation free radical initiating system and method for preparing hydrogel by using glucose oxidase mediation free radical initiating system |
| CN105254812A (en) * | 2015-11-11 | 2016-01-20 | 江南大学 | Grafted starch slurry preparation method based on enzymatic cascade reaction |
| CN105732900A (en) * | 2016-04-14 | 2016-07-06 | 安徽农业大学 | Super absorbent resin containing boron and preparing method thereof |
| CN105801753A (en) * | 2016-04-14 | 2016-07-27 | 安徽农业大学 | Method for preparing high-water-absorption resin with biological enzyme as catalytic initiator |
| CN105859967A (en) * | 2016-04-14 | 2016-08-17 | 安徽农业大学 | High water-absorbing resin containing iron ions and preparation method thereof |
| CN105859966A (en) * | 2016-04-14 | 2016-08-17 | 安徽农业大学 | High water-absorbing resin containing zinc element and a preparation method thereof |
| CN106087110A (en) * | 2016-06-28 | 2016-11-09 | 郭迎庆 | A kind of preparation method of starch sugar crosslinking flax fiber |
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| CN105239387B (en) * | 2015-11-11 | 2018-09-28 | 江南大学 | A kind of method that full biological enzyme prepares high-performance environment-friendly spinning sizing agent |
| CN113024897A (en) * | 2021-03-10 | 2021-06-25 | 杭州纸友科技有限公司 | Preparation method of high-strength TPS starch for degradable material |
| CN113358598A (en) * | 2021-05-26 | 2021-09-07 | 四川农业大学 | Method for rapidly determining amylose content of wheat crops based on iodine dyeing method |
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| CN103436572A (en) * | 2013-08-14 | 2013-12-11 | 江南大学 | Preparation method of tubular starch derivative |
| CN104418971A (en) * | 2013-09-09 | 2015-03-18 | 同济大学 | Glucose oxidase mediation free radical initiating system and method for preparing hydrogel by using glucose oxidase mediation free radical initiating system |
| CN104418971B (en) * | 2013-09-09 | 2016-07-13 | 同济大学 | Glucoseoxidase mediation free radical initiator system and the method preparing hydrogel thereof |
| CN105254812A (en) * | 2015-11-11 | 2016-01-20 | 江南大学 | Grafted starch slurry preparation method based on enzymatic cascade reaction |
| CN105239387B (en) * | 2015-11-11 | 2018-09-28 | 江南大学 | A kind of method that full biological enzyme prepares high-performance environment-friendly spinning sizing agent |
| CN105859967A (en) * | 2016-04-14 | 2016-08-17 | 安徽农业大学 | High water-absorbing resin containing iron ions and preparation method thereof |
| CN105801753A (en) * | 2016-04-14 | 2016-07-27 | 安徽农业大学 | Method for preparing high-water-absorption resin with biological enzyme as catalytic initiator |
| CN105859966A (en) * | 2016-04-14 | 2016-08-17 | 安徽农业大学 | High water-absorbing resin containing zinc element and a preparation method thereof |
| CN105732900A (en) * | 2016-04-14 | 2016-07-06 | 安徽农业大学 | Super absorbent resin containing boron and preparing method thereof |
| CN106087110A (en) * | 2016-06-28 | 2016-11-09 | 郭迎庆 | A kind of preparation method of starch sugar crosslinking flax fiber |
| CN108102148A (en) * | 2017-12-29 | 2018-06-01 | 江南大学 | A kind of processing method of high-barrier bacteriostatic starch based composites |
| CN108102148B (en) * | 2017-12-29 | 2019-09-03 | 江南大学 | A kind of processing method of high-barrier bacteriostatic starch based composites |
| CN113024897A (en) * | 2021-03-10 | 2021-06-25 | 杭州纸友科技有限公司 | Preparation method of high-strength TPS starch for degradable material |
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