CN103571649B - Oxidized starch-based compound detergent auxiliary and preparation method thereof - Google Patents
Oxidized starch-based compound detergent auxiliary and preparation method thereof Download PDFInfo
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- CN103571649B CN103571649B CN201310318280.6A CN201310318280A CN103571649B CN 103571649 B CN103571649 B CN 103571649B CN 201310318280 A CN201310318280 A CN 201310318280A CN 103571649 B CN103571649 B CN 103571649B
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Abstract
The invention relates to the field of starch modification, and in particular to an oxidized starch-based compound detergent auxiliary and a preparation method thereof. The oxidized starch-based compound detergent auxiliary comprises the following components in weight proportion: 100g of starch, 5-15g of oxidant and 10-30g of dispersant. The preparation method comprises the following steps: weighing the starch, the oxidant and the dispersant according to the weight proportion of the components of the oxidized starch-based compound detergent auxiliary, uniformly mixing and placing in a ball mill, enabling the starch to synchronously oxidize and compound with the oxidant and the dispersant when the stirring speed in the ball mill is 100-250rpm and the temperature is 30-80 DEG.C, reacting for 20-90 minutes, and then drying to obtain the oxidized starch-based compound detergent auxiliary. The carboxyl content of the product is 0.8-2.5%, and is improved by 20-30% in comparison with the prior art, the production is sufficient in reaction, the yield is high, and the preparation process is simple.
Description
Technical field
The invention belongs to field of starch modification, specifically a kind of Sumstar 190 base compound detergent auxiliary and preparation method thereof.
Background technology
Tripoly phosphate sodium STPP causes the concern in the whole world as the water source extensive use of chemical fertilizer phenomenon that washing auxiliary detergent causes, the washing auxiliary detergent that can replace tripoly phosphate sodium STPP is actively being found always by various countries, such as 4A zeolite, lamina sodium silicate, Starso etc., these washing assistants respectively have oneself relative merits, are not more desirable washing assistants with tripoly phosphate sodium STPP.The wide material sources of starch, cheap, biodegradable, it is a kind of reproducible industrial raw material, Sumstar 190 is a kind of modified starch, existing Research foundation finds Sumstar 190 has certain washing aid performance, is expected to be applied in detergent applications as washing auxiliary detergent.The metal ions such as Sumstar 190 energy complexing calcium, magnesium, make water softening and can adsorb, disperse, the performance of soil suspension, develop it as non-phosphorus washing assistant to replace STPP, reach and reduce phosphorus content in water, prevention Water Eutrophication will be one and significantly work, existing following progress.
The people such as Zhang Yanping take W-Gum as raw material, are that oxygenant has been prepared high-carboxyl-content Sumstar 190 and have studied its washing aid performance with clorox, find that Sumstar 190 increases along with the increase of carboxyl-content the huge legendary turtle of calcium ion ability of closing.Meanwhile, Sumstar 190 is to solids foul MnO
2suspended dispersed ability strengthen along with the increase of carboxyl-content.With the helping to wash in contrast experiment and also find of polyphosphoric acid salt, high oxidized starch is to simulation solids foul MnO
2suspended dispersed and dispersion stabilization be all better than polyphosphoric acid salt.
King to sew with long stitches etc. at alkali, oxygen and under the effect of controlling catalyst, prepares W-Gum oxide compound, and best manufacturing condition is: catalyzer (in W-Gum) is 1.4 ~ 1.8%; Temperature of reaction is 100 DEG C; Reaction times is 3.5h; Oxygen-supply quantity is 550 ~ 650mL/h.The maize oxidized starch hydrolyzate of this explained hereafter, has the ability of certain complexing calcium ions, can be used as washing auxiliary detergent formulated non-phosphide detergent.
Jiang Wen is brave etc. utilizes calcium ion-selective electrode and the complex ability of chemical analysis to starch oxidation thing to measure.Investigate the impact of Sumstar 190 add-on, pH value and temperature on calcium complex ability.Result shows, under experimental conditions, temperature raises, and the complex ability of Sumstar 190 increases, 35 DEG C time, reach maximum value; Be in 9 ~ 10 scopes in pH value, along with pH value increases, complex ability increase is less, reaches maximum value when pH=9.8; Along with the increase of Sumstar 190 add-on, the complex ability of Sumstar 190 increases, and when the massfraction added is more than 0.02, the complex ability of the W-Gum oxide compound of unit vol declines, and the complexing amount of starch oxidation thing to calcium ion can reach 92.25mg/g.
Wang Qiuhua with appropriate from controlling catalyst, oxygen is oxygenant, be 100g, NaOH consumption at starch consumption be 21g, prepare a kind of new type water-solubility degree of depth maize oxidized starch under temperature of reaction 100 DEG C, reaction times 3.0h condition, find that the ability of this Sumstar 190 complexing calcium ions reaches 104.5mg/g, and have good decontamination ratio.
Sumstar 190 is very easily degraded by microorganisms in physical environment, and its biological degradability is higher than other macromolecular compound.Used as washing auxiliary detergent, environmentally friendly, simultaneously cheap, resource is renewable, functional, is therefore expected the ideal substitute becoming STPP.But starch has the grain pattern of crystallization, inside is noncrystalline domain, and outside is crystallizing field and very firmly, has stronger resistivity to water and chemical reagent.Sumstar 190 degree of oxidation obtained by existing Sumstar 190 preparation method is lower, and solubleness is weak, makes it in washing auxiliary detergent application, be subject to a definite limitation.Therefore, how according to the embody rule needs of product, suitable method is selected to carry out pre-treatment to starch, change the grain pattern of starch and reduce starch crystals district, improve its chemical reactivity, improve its solubleness and oxidation effectiveness, the obtained oxygenated products conforming with washing needs has problem to be solved at present.
Summary of the invention
The object of the invention is to overcome existing Sumstar 190 as washing auxiliary detergent exist preparation time long, react insufficient, the problem such as complex procedures, performance are single, solubleness is low, carboxyl-content is low, chelating calcium ion ability is low, a kind of Sumstar 190 base compound detergent auxiliary and preparation method thereof is provided.
The solution of the present invention is by realizing like this: a kind of Sumstar 190 base compound detergent auxiliary, the raw material preparing this Sumstar 190 base compound detergent auxiliary comprises starch, oxygenant, washing assistant, preparing each raw material of this Sumstar 190 base compound detergent auxiliary is 100g:5 ~ 15g:10 ~ 30g according to the part by weight of starch, oxygenant, washing assistant, prepares through synchronous oxidizing reaction and complex role.
As further restriction of the present invention, above-described starch is any one or their mixture in tapioca (flour), W-Gum, and its size is 40 ~ 100 orders; Described oxygenant is potassium permanganate KMnO
4, clorox NaClO, oxydol H
2o
2, ammonium sulfate (NH
4)
2sO
4, Peracetic Acid C
2h
4o
3in any one or their mixture; Described washing assistant is 4A zeolite Na
12al
12si
12o
4827H
2any one or their mixture in O, lamina sodium silicate, polyacrylic acid, Starso.Starch preferred version of the present invention is tapioca (flour), and oxygenant preferred version is oxydol H
2o
2, potassium permanganate KMnO
4, Peracetic Acid C
2h
4o
3in any one, washing assistant preferred version is 4A zeolite Na
12al
12si
12o
4827H
2any one in O, lamina sodium silicate.
A kind of method preparing Sumstar 190 base compound detergent auxiliary, be 100g:5 ~ 15g:10 ~ 30g according to the part by weight of starch, oxygenant, washing assistant, take starch, oxygenant, washing assistant respectively, three's mixing is placed in ball mill, in ball mill, stirring velocity is 100-250rpm, temperature is make starch and oxygenant, washing assistant that oxygenizement and complex role synchronously occur under 30-80 DEG C of condition, carry out drying after reaction 20-90min, obtain Sumstar 190 base compound detergent auxiliary product.When wherein carrying out Simultaneous Oxidation reaction and complex role in ball mill, as required according to material (starch, oxygenant, washing assistant summation): grinding media is that the ratio of 100g:300mL carries out mix and blend, improve mechanical activation efficiency.
The know-why that the present invention realizes is: prepare Sumstar 190 base Compositional type washing auxiliary detergent by utilizing this emerging interleaving techniques of mechanical activation, purposes that can be different according to it, choose the starch of suitable proportion, oxygenant, washing assistant, by the composite modified degree of the oxidation adjusting mechanical soak time, temperature controls starch, the oxidising process of starch and composite modified process are carried out simultaneously, simplifies preparation section.Mechanical activation technology can change the grain pattern of starch and reduce starch crystals district, material in reaction process is fully contacted, reaction reaches abundant, reaction product carboxyl-content reaches 0.8 ~ 2.5%, mechanical activation effect simultaneously greatly can improve product solubility, shorten the time of reaction, simplify preparation technology.And utilize washing assistant such as 4A zeolite, lamina sodium silicate etc. to carry out composite with Sumstar 190, reaction product is made not only to have excellent solvability, there is again the premium properties of Sumstar 190 self, there is the good characteristics of washing assistant itself simultaneously, composite result makes its complexing calcium, the ability of magnesium ion is improved significantly.
As further restriction of the present invention, the above drying is dry Sumstar 190 base compound detergent auxiliary under 40-60 DEG C of condition, makes its moisture content be 2 ~ 10%.
As further restriction of the present invention, the above starch preparing in Sumstar 190 base compound detergent auxiliary method is any one or their mixture in tapioca (flour), W-Gum, and its size is 40 ~ 100 orders; Described oxygenant is potassium permanganate KMnO
4, clorox NaClO, oxydol H
2o
2, ammonium sulfate (NH
4)
2sO
4, Peracetic Acid C
2h
4o
3in any one or their mixture; Described washing assistant is 4A zeolite Na
12al
12si
12o
4827H
2any one or their mixture in O, lamina sodium silicate, polyacrylic acid, Starso.Starch preferred version of the present invention is tapioca (flour), and oxygenant preferred version is oxydol H
2o
2, potassium permanganate KMnO
4, Peracetic Acid C
2h
4o
3in any one, washing assistant preferred version is 4A zeolite Na
12al
12si
12o
4827H
2any one in O, lamina sodium silicate.
The present invention possesses following good result:
(1) the present invention utilizes mechanical activation process to make starch, under the katalysis of oxygenant, oxidizing reaction occur, obtain carboxyl-content in the finished product to improve, carboxyl can with the calcium in hard water, magnesium ion sequestration, form inner complex that is stable, solubility and give removing, carboxyl-content improves it and also increases the interdiction capacity of calcium, magnesium ion, final reduction water hardness, reduces calcium soap and generates, have the performance of softening water.In addition, the Sumstar 190 that Sumstar 190 base compound detergent auxiliary is relatively conventional unmodified, has that gelatinization point is low, viscosity is low, good film-forming property, cohesiveness are good, anticoagulant and a premium properties such as the transparency is good.For single washing assistant as 4A zeolite Na
12al
12si
12o
4827H
2o, lamina sodium silicate, polyacrylic acid, Starso etc. have more excellent compound property.
(2) the present invention's product carboxyl-content of adopting phenolphthalein variable color method to detect the present invention to prepare, product carboxyl-content is 0.8%-2.5%, improve 20 ~ 38% relative to prior art level, the raising of carboxyl-content makes Sumstar 190 suppress the ability of calcium carbonate crystal synchronously to get a promotion to the complex ability of calcium ion, Sumstar 190 dispersing property, Sumstar 190, compared with starting material starch, existing Sumstar 190, its character there occurs very large change.
(3) the mechanical activation technology that the present invention adopts can change the grain pattern of starch and reduce starch crystals district, material in reaction process is fully contacted, reaction reaches abundant, reaction product carboxyl-content reaches 0.8 ~ 2.5%, mechanical activation effect simultaneously greatly can improve product solubility, shorten the time of reaction, simplify preparation technology.
Accompanying drawing explanation
Fig. 1. Sumstar 190 base compound detergent auxiliary preparation method schema.
Embodiment
Describe a kind of Sumstar 190 base of the present invention compound detergent auxiliary and preparation method thereof below in conjunction with embodiment and accompanying drawing, these descriptions are not be further limited content of the present invention.
Embodiment 1
The present embodiment Sumstar 190 base compound detergent auxiliary moiety tapioca (flour), Peracetic Acid C
2h
4o
3oxygenant, 4A zeolite Na
12al
12si
12o
4827H
2the part by weight of O washing assistant is 100g:10g:15g, three's mixing is placed in ball mill, and according to material (starch, oxygenant, washing assistant weight summation): the ratio of grinding media=100g:300mL adds grinding media, in ball mill, stirring velocity is 100rpm, temperature is make starch and oxygenant, washing assistant that oxygenizement and complex role synchronously occur under 50 DEG C of conditions, after reaction 40min, drying is carried out under 40 DEG C of conditions, make its moisture content be 8%, Sumstar 190 base compound detergent auxiliary product can be obtained.In the present embodiment, granule size controls is 40 orders.
The Sumstar 190 base compound detergent auxiliary 0.500g that the present embodiment obtains, carry out washing through 95% ethanol and remove chlorion, boil 5-7min again, with phenolphthalein as indicator, titration NaOH standardized solution is to phenolphthalein variable color, the volume V of record NaOH, utilizes the relation between the volume V of NaOH and the quality of working sample consumed, and calculating the carboxyl amount that the present embodiment obtains product is 1.2%.It is 150mg/g that the present embodiment obtains product complexing calcium ions ability.
Embodiment 2
The present embodiment Sumstar 190 base compound detergent auxiliary moiety tapioca (flour), W-Gum, Peracetic Acid C
2h
4o
3oxygenant, oxydol H
2o
2oxygenant, lamina sodium silicate washing assistant, the part by weight of Starso washing assistant is 50g:50g:10g:5g:10g:5g, three's mixing is placed in ball mill, and according to material (starch, oxygenant, washing assistant weight summation): the ratio of grinding media=100g:300mL adds grinding media, in ball mill, stirring velocity is 150rpm, temperature is make starch and oxygenant under 80 DEG C of conditions, synchronously there is oxygenizement and complex role in washing assistant, after reaction 50min, drying is carried out under 50 DEG C of conditions, its moisture content is made to be 7%, Sumstar 190 base compound detergent auxiliary product can be obtained.In the present embodiment, granule size controls is 50 orders.
The Sumstar 190 base compound detergent auxiliary 0.500g that the present embodiment obtains, carry out washing through 95% ethanol and remove chlorion, boil 5-7min again, with phenolphthalein as indicator, titration NaOH standardized solution is to phenolphthalein variable color, the volume V of record NaOH, utilizes the relation between the volume V of NaOH and the quality of working sample consumed, and calculating the carboxyl amount that the present embodiment obtains product is 2.0%.It is 120mg/g that the present embodiment obtains product complexing calcium ions ability.
Embodiment 3
The present embodiment Sumstar 190 base compound detergent auxiliary moiety tapioca (flour), potassium permanganate KMnO
4oxygenant, polyacrylic acid washing assistant, 4A zeolite Na
12al
12si
12o
4827H
2the part by weight of O washing assistant is 100g:5g:20g:5g, three's mixing is placed in ball mill, and according to material (starch, oxygenant, washing assistant weight summation): the ratio of grinding media=100g:300mL adds grinding media, in ball mill, stirring velocity is 200rpm, temperature is make starch and oxygenant, washing assistant that oxygenizement and complex role synchronously occur under 60 DEG C of conditions, after reaction 55min, drying is carried out under 50 DEG C of conditions, make its moisture content be 5%, Sumstar 190 base compound detergent auxiliary product can be obtained.In the present embodiment, granule size controls is 60 orders.
The Sumstar 190 base compound detergent auxiliary 0.500g that the present embodiment obtains, carry out washing through 95% ethanol and remove chlorion, boil 5-7min again, with phenolphthalein as indicator, titration NaOH standardized solution is to phenolphthalein variable color, the volume V of record NaOH, utilizes the relation between the volume V of NaOH and the quality of working sample consumed, and calculating the carboxyl amount that the present embodiment obtains product is 1.5%.It is 100mg/g that the present embodiment obtains product complexing calcium ions ability.
Embodiment 4
The present embodiment Sumstar 190 base compound detergent auxiliary moiety W-Gum, clorox NaClO oxygenant, the part by weight of Starso washing assistant is 100g:8g:10g, three's mixing is placed in ball mill, and according to material (starch, oxygenant, washing assistant weight summation): the ratio of grinding media=100g:300mL adds grinding media, in ball mill, stirring velocity is 150rpm, temperature is make starch and oxygenant under 40 DEG C of conditions, synchronously there is oxygenizement and complex role in washing assistant, under 60 DEG C of conditions, drying is carried out after reaction 60min, its moisture content is made to be 4%, Sumstar 190 base compound detergent auxiliary product can be obtained.In the present embodiment, granule size controls is 40 orders.
The Sumstar 190 base compound detergent auxiliary 0.500g that the present embodiment obtains, carry out washing through 95% ethanol and remove chlorion, boil 5-7min again, with phenolphthalein as indicator, titration NaOH standardized solution is to phenolphthalein variable color, the volume V of record NaOH, utilizes the relation between the volume V of NaOH and the quality of working sample consumed, and calculating the carboxyl amount that the present embodiment obtains product is 0.8%.It is 125mg/g that the present embodiment obtains product complexing calcium ions ability.
Embodiment 5
The present embodiment Sumstar 190 base compound detergent auxiliary moiety tapioca (flour), W-Gum, ammonium sulfate (NH
4)
2sO
4the part by weight of oxygenant, lamina sodium silicate washing assistant is 80g:20g:12g:20g, three's mixing is placed in ball mill, and according to material (starch, oxygenant, washing assistant weight summation): the ratio of grinding media=100g:300mL adds grinding media, in ball mill, stirring velocity is 250rpm, temperature is make starch and oxygenant, washing assistant that oxygenizement and complex role synchronously occur under 70 DEG C of conditions, under 60 DEG C of conditions, drying is carried out after reaction 90min, make its moisture content be 10%, Sumstar 190 base compound detergent auxiliary product can be obtained.In the present embodiment, granule size controls is 100 orders.
The Sumstar 190 base compound detergent auxiliary 0.500g that the present embodiment obtains, carry out washing through 95% ethanol and remove chlorion, boil 5-7min again, with phenolphthalein as indicator, titration NaOH standardized solution is to phenolphthalein variable color, the volume V of record NaOH, utilizes the relation between the volume V of NaOH and the quality of working sample consumed, and calculating the carboxyl amount that the present embodiment obtains product is 2.5%.It is 130mg/g that the present embodiment obtains product complexing calcium ions ability.
Embodiment 6
The present embodiment Sumstar 190 base compound detergent auxiliary moiety tapioca (flour), W-Gum, oxydol H
2o
2the part by weight of oxygenant, polyacrylic acid washing assistant is 60g:40g:10g:30g, three's mixing is placed in ball mill, and according to material (starch, oxygenant, washing assistant weight summation): the ratio of grinding media=100g:300mL adds grinding media, in ball mill, stirring velocity is 100rpm, temperature is make starch and oxygenant, washing assistant that oxygenizement and complex role synchronously occur under 30 DEG C of conditions, under 50 DEG C of conditions, drying is carried out after reaction 20min, make its moisture content be 9%, Sumstar 190 base compound detergent auxiliary product can be obtained.In the present embodiment, granule size controls is 80 orders.
The Sumstar 190 base compound detergent auxiliary 0.500g that the present embodiment obtains, carry out washing through 95% ethanol and remove chlorion, boil 5-7min again, with phenolphthalein as indicator, titration NaOH standardized solution is to phenolphthalein variable color, the volume V of record NaOH, utilizes the relation between the volume V of NaOH and the quality of working sample consumed, and calculating the carboxyl amount that the present embodiment obtains product is 1.8%.It is 140mg/g that the present embodiment obtains product complexing calcium ions ability.
The above embodiment of the present invention scheme is only can not limit the present invention to explanation of the present invention, the scope of product moiety of the present invention, component proportions, preparation method's parameter is indicated in claim, and the scope of parameter of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, is all considered to be and is included in the scope of claims.
The present invention is through multidigit Sumstar 190 and washing assistant processing staff long term operation experience accumulation, and created by creative work, product carboxyl-content of the present invention is 0.8%-2.5%, improve 20 ~ 38% relative to prior art level, the raising of carboxyl-content makes Sumstar 190 suppress the ability of calcium carbonate crystal synchronously to get a promotion to the complex ability of calcium ion, Sumstar 190 dispersing property, Sumstar 190, compared with starting material starch, existing Sumstar 190, its character there occurs very large change.
Claims (4)
1. a Sumstar 190 base compound detergent auxiliary, the raw material preparing this Sumstar 190 base compound detergent auxiliary comprises starch, oxygenant, washing assistant, it is characterized in that, preparing each raw material of this Sumstar 190 base compound detergent auxiliary is 100g:5 ~ 15g:10 ~ 30g according to the part by weight of starch, oxygenant, washing assistant, prepares through synchronous oxidizing reaction and complex role;
Described oxygenant is potassium permanganate KMnO
4, clorox NaClO, oxydol H
2o
2, ammonium sulfate (NH
4)
2sO
4, Peracetic Acid C
2h
4o
3in any one or their mixture; Described washing assistant is 4A zeolite Na
12al
12si
12o
4827H
2any one or their mixture in O, lamina sodium silicate, polyacrylic acid, Starso.
2. Sumstar 190 base compound detergent auxiliary according to claim 1, is characterized in that, described starch is any one or their mixture in tapioca (flour), W-Gum, and its size is 40 ~ 100 orders.
3. prepare the method for the Sumstar 190 base compound detergent auxiliary described in any one of claim 1 or 2 for one kind, it is characterized in that, according to starch, oxygenant, the part by weight of washing assistant is 100g:5 ~ 15g:10 ~ 30g, take starch respectively, oxygenant, washing assistant, three's mixing is placed in ball mill, in ball mill, stirring velocity is 100-250rpm, temperature is make starch under 30-80 DEG C of condition, synchronously there is oxidizing reaction and complex role in oxygenant and washing assistant, drying is carried out after reaction 20-90min, obtain Sumstar 190 base compound detergent auxiliary product,
Described starch is any one or their mixture in tapioca (flour), W-Gum, and its size is 40 ~ 100 orders; Described oxygenant is potassium permanganate KMnO
4, clorox NaClO, oxydol H
2o
2, ammonium sulfate (NH
4)
2sO
4, Peracetic Acid C
2h
4o
3in any one or their mixture; Described washing assistant is 4A zeolite Na
12al
12si
12o
4827H
2any one or their mixture in O, lamina sodium silicate, polyacrylic acid, Starso.
4. the method preparing Sumstar 190 base compound detergent auxiliary according to claim 3, is characterized in that, described drying is dry Sumstar 190 base compound detergent auxiliary under 40-60 DEG C of condition, makes its moisture content be 2 ~ 10%.
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| CN103571649B true CN103571649B (en) | 2015-04-08 |
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| CN100503641C (en) * | 2007-01-25 | 2009-06-24 | 天津科技大学 | Natural organism coagulant aid and preparing method theroef |
| CN103012605B (en) * | 2012-12-11 | 2015-01-14 | 广西民族大学 | Method for preparing high-retention environmental-friendly one-step double-modified starch |
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