CN103333306A - Preparation method of water-soluble polyurethane graft starch water treatment agent - Google Patents
Preparation method of water-soluble polyurethane graft starch water treatment agent Download PDFInfo
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- CN103333306A CN103333306A CN2013102969689A CN201310296968A CN103333306A CN 103333306 A CN103333306 A CN 103333306A CN 2013102969689 A CN2013102969689 A CN 2013102969689A CN 201310296968 A CN201310296968 A CN 201310296968A CN 103333306 A CN103333306 A CN 103333306A
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Abstract
The invention belongs to the technical field of water treatment agents and particularly relates to a preparation method of a water-soluble polyurethane graft starch water treatment agent. The preparation method is characterized by comprising the following steps: 1) weighting starch and measuring water in the weight ratio of 1 to 9, and stirring the starch and the water; 2) warming to 90 DEG C, regulating pH to 10 to 11; 3) weighting urea in molar ration that the urea to starch is 1 to 1, and then stirring, so as to obtain a mixture A; 4) measuring formaldehyde solution and weighting urea in molar ration that the starch to formaldehyde solution to urea is (1 to 1 to 1) to (1 to 15 to 15); 5) regulating the pH of formaldehyde solution to 6 to 8 by hydrochloric acid and then adding urea to formaldehyde solution, so as to obtain a mixture B; 6) dropping the mixture A into the mixture B and stirring, so as to obtain a mixture C; 7) measuring formaldehyde solution and dimethylamine in molar ration that starch to formaldehyde solution to dimethylamine is (1 to 1 to 1) to (1 to 15 to 15), adding the formaldehyde solution and dimethylamine into the mixture C, and regulating the pH of mixture C to 6.5 to 7.5, so as to obtain liquid product D; 8) drying the liquid product D, so as to obtain solid water-soluble polyurethane graft starch water treatment agent. The water treatment agent prepared by the method has a better flocculation effect.
Description
Technical field
The invention belongs to the water conditioner technical field, be specifically related to a kind of preparation method of water-soluble polyurethane graft starch water conditioner.
Background technology
China's Freshwater resources are limited, and the water resources occupied area is few per capita.The increase of population, expanding economy and quickening of urbanization process, shortage of water resources, water is seriously polluted, the unbalanced situation of water distribution is more severe.The purifying treatment of sewage is the important measures of water saving.In the numerous water technology, be the treatment process most widely used, that cost is minimum and the most frequently used with flocculent precipitation now.Main flocculation agent has anionic/cationic/non-ionic polyacrylamide, aluminium, iron zinc salt and polymkeric substance etc., and they all have good effect, but have the hidden danger of secondary pollution.Starch contains a plurality of hydroxyls, on these activity hydroxy groups, introduce monomer, grafting, copolymerization, crosslinked and etherification reaction can take place under the certain condition, the preparation treated starch, wherein partially modified starch be applied to water quality purification [Zhan Yali Guo Shao brightness Lv Rong lake. research and the application of green reagent starch conversion water conditioner. polymer material science and engineering .2003,19(5): 14-18].Be development of raw materials green, efficient and degradable water conditioner with starch, be still the important development direction of following water conditioner.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of water-soluble polyurethane graft starch water conditioner, the water conditioner of this method preparation has flocculating effect preferably.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of water-soluble polyurethane graft starch water conditioner is characterized in that it comprises the steps:
1) by starch: the weight ratio of water=1:9 takes by weighing starch, measures water, and water and starch are stirred, and obtains the mixture of starch and water;
2) be warming up to the mixture (gelatinization 5-10 minute, namely be incubated 5-10 minute, color is become the transparent color of thickness by oyster white) of 90 ℃ of pasted starches and water, and add NaOH solution and regulate pH to 10-11, the starch paste of adjusted good pH;
3) by urea: the mol ratio of starch=1:1 takes by weighing urea, joins step 2) in regulate in the starch paste of pH, stir, be warming up to 95-97 ℃, insulation 1-2h transfers pH to 4.8-5.4 with hydrochloric acid (HCl), gets mixture A;
4) according to starch: the mol ratio of formaldehyde solution: urea=1:1:1-1:15:15 is measured formaldehyde solution (being formalin), takes by weighing urea, and the concentration of described formaldehyde solution is the 37wt% formalin;
5) transfer the pH to 6-8 of formaldehyde solution with hydrochloric acid (HCl), in formaldehyde solution (being formalin), add urea then, be warmed up to 90-95 ℃ (slowly heat up, slowly refer to temperature rise rate be 1 ℃/min), insulation 2h gets mixture B;
6) the mixture B that the mixture A that step 3) is obtained and step 5) obtain, by mixture A: the mol ratio of mixture B=1:1-1:15 is got mixture A and mixture;
Mixture B splashed among the mixture A (drip off in the 30min), stir, and keep 90 ℃ of temperature, drip off afterreaction 40-60min, be cooled to 40 ℃, get mixture C;
7) according to starch: formaldehyde solution: the ratio of the mol ratio=1:1:1-1:15:15 of dimethylamine is measured formaldehyde solution (being formalin) and dimethylamine, join simultaneously in the mixture C that step 6) obtains, 40 ℃, stir, insulation 2h, regulate pH=6.5-7.5 with hydrochloric acid (HCl), get liquid product D; The concentration of described formaldehyde solution is the 37wt% formalin;
8) with liquid product drying (with 60 ℃ of forced air dryings), namely get the water-soluble polyurethane graft starch water conditioner of solid.
The concentration of described NaOH solution (the NaOH aqueous solution) is 10-30wt%.
The concentration of described hydrochloric acid is 10-30wt%.
In the step 4), according to starch: the mol ratio of formaldehyde solution: urea=1:7.5:7.5 is measured formaldehyde solution, takes by weighing urea.
In the step 7), according to starch: formaldehyde solution: the ratio of the mol ratio=1:7.5:7.5 of dimethylamine is measured formaldehyde solution and dimethylamine.
The invention has the beneficial effects as follows: the water conditioner of this method preparation has flocculating effect preferably, dispensing dosage is under 5mg/L concentration, pH there is good flocculating effect at the 0.5wt% of 5-8 bentonite suspension, can clarify the suspension of 85% volume during flocculation 3min, flocculation (clarification) speed is fast, and flocculating effect is good.
The present invention can be used for conglomerate sewage purification such as tap water processing and sanitary sewage, papermaking wastewater, textile sewage and recycles, and substitutes existing acrylic amide water conditioner, for China's water surrounding purification industry provides new product of environment protect.
Description of drawings
Fig. 1 is the infrared spectrogram of water-soluble polyurethane graft starch water conditioner of the present invention.
Fig. 2 is that water-soluble polyurethane graft starch water conditioner of the present invention is to the flocculating effect figure of bentonite suspension.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
A kind of preparation method of water-soluble polyurethane graft starch water conditioner, it comprises the steps:
1) by starch: the weight ratio of water=1:9 takes by weighing starch 10g, measures water 90mL(distilled water), and water and starch stirred (in three mouthfuls of round-bottomed flasks that electronic stirring, water condensation and water bath with thermostatic control be housed) obtain the mixture of starch and water;
2) be warming up to the mixture of 90 ℃ of pasted starches and water, insulation 10min with starch pasting (obtaining starch paste), and adds the NaOH solution that 0.2 mL concentration is 10wt% (the NaOH aqueous solution) and regulates pH to 10, the starch paste of adjusted good pH;
3) by urea: the mol ratio of starch=1:1 takes by weighing urea 4.07g, joins step 2) in regulate in the starch paste of pH, stir, be warming up to 95 ℃, insulation 1h transfers pH to 4.8 with hydrochloric acid (HCl), gets mixture A; The concentration of described hydrochloric acid is 10-30wt%;
4) according to starch: the mol ratio of formaldehyde solution: urea=1:1:1 is measured formaldehyde solution (being formalin) 6.8mL, takes by weighing urea 4.07g, and wherein the concentration of formaldehyde solution (being formalin) is 37wt%;
5) another electronic stirring, water condensation and water bath with thermostatic control there-necked flask in, transfer the pH to 6 of formaldehyde solution with hydrochloric acid (HCl), in formaldehyde solution, add urea then, slowly be warmed up to 90 ℃ (slowly refer to temperature rise rate be 1 ℃/min), insulation 2h, pour in the separating funnel, get mixture B; The concentration of described hydrochloric acid is 10-30wt%;
6) the mixture B that step 5) is obtained packs into together with separating funnel in three mouthfuls of round-bottomed flasks (there-necked flask) that mixture A is housed that step 3) obtains, stir, and keep 90 ℃ of temperature, open the separating funnel piston, guarantee in 30min, to drip mixture B in mixture A, react 40-60min after dripping again, be cooled to 40 ℃, get mixture C;
7) according to starch: formaldehyde solution: the ratio of the mol ratio=1:1:1 of dimethylamine is measured formaldehyde solution (being formalin) 6.8 mL and dimethylamine 11mL, join simultaneously in the mixture C that step 6) obtains, 40 ℃, stir, insulation 2h, regulate pH=6.5 with hydrochloric acid (HCl), get liquid product D; Wherein the concentration of formaldehyde solution (being formalin) is 37wt%;
8) with liquid product D with 60 ℃ of forced air dryings, namely get the water-soluble polyurethane graft starch water conditioner of solid.
With water-soluble polyurethane graft starch water conditioner (product) and the pressing potassium bromide troche of present embodiment, do Infrared spectroscopy.Infrared spectrogram is seen Fig. 1:
Known starch is at 575.9 cm
-1, 765.1 cm
-1, 860.7 cm
-1With 3396.0 cm
-1Be characteristic peak-CH
2-and-wavelength of OH-correspondence.Water-soluble polyurethane graft starch water conditioner (product) is at 3409.2 cm among this figure
-1The place has-OH and-NH stretching vibration, at 1641.3cm
-1There are the flexible peak of acid amides C=O and 1247.5 cm in the place
-1The acid amides III bands of a spectrum that place's C-N-H vibration produces.
The result shows: urethane and starch success grafting.
The flocculating effect experiment:
1) gets the 0.5g wilkinite, add and be equipped with in the tool plug graduated measuring glass cylinder of 100 mL water, be made into the bentonite suspension of 0.5wt% concentration.Totally 5 parts, number 1-5 number, wherein be contrast No. 1;
2) accurately take by weighing 0.500 mg water-soluble polyurethane graft starch water conditioner (product), totally 4 parts;
3) in the 2-5 bentonite suspension, add step 2) ready water conditioner (contrast does not add), begin immediately to stir, the 1-5 churning time is respectively 4,1,2,3,4min, and guarantees that stirring stops simultaneously.
4) after stirring finishes, leave standstill, every interval certain hour is observed the sedimentation situation of solution in the graduated cylinder, and takes pictures;
5) compare churning time to the influence of water conditioner flocculating effect.
Four kinds of churning time are little to the flocculating effect influence of water conditioner, but time of repose is influential.The 2-5 graduated cylinder all shows as: occur significantly flocculation interface in the time of repose of 2min, the clarified liq volume has reached 80-82 mL when 5min, and after this prolongation clarification volume change in time is little.And No. 1 reach the clarification volume that 80 mL just appear in 40min to impinging upon, and mainly is the result of natural subsidence.Effect of settling is seen Fig. 2.
The result shows: water-soluble polyurethane graft starch water conditioner has flocculating effect preferably.
Embodiment 2:
A kind of preparation method of water-soluble polyurethane graft starch water conditioner, it comprises the steps:
1) by starch: the weight ratio of water=1:9 takes by weighing starch 10g, measures water 90mL(distilled water), and water and starch stirred, the mixture of starch and water obtained;
2) be warming up to the mixture (be incubated 10 min, obtain starch paste) of 90 ℃ of pasted starches and water, and to add concentration be that the NaOH solution of 10wt% is regulated pH to 11(and also can be adopted the NaOH solution of 30wt% to regulate pH to 11), the starch paste of adjusted good pH;
3) by urea: the mol ratio of starch=1:1 takes by weighing urea 4.07 gram, joins step 2) in regulate in the starch paste of pH, stir, be warming up to 97 ℃, insulation 2h transfers pH to 5.4 with hydrochloric acid, gets mixture A; The concentration of described hydrochloric acid is 10-30wt%;
4) according to starch: the mol ratio of formaldehyde solution: urea=1:15:15 is measured formaldehyde solution (being formalin) 102 mL, takes by weighing urea 61.05g, and wherein the concentration of formaldehyde solution (being formalin) is 37wt%;
5) transfer the pH to 8 of formalin with hydrochloric acid (HCl), in formalin, add urea then, slowly be warmed up to 95 ℃ (slowly refer to temperature rise rate be 1 ℃/min), insulation 2h pours in the separating funnel, gets mixture B; The concentration of described hydrochloric acid is 10-30wt%;
6) after mixture A is warming up to 90 ℃, mixture B slowly is added drop-wise among the mixture A (drips in the 30min), stir (and keeping 90 ℃ of temperature), reaction 40-60min is cooled to 40 ℃, gets mixture C;
7) according to starch: formaldehyde solution: the ratio of the mol ratio=1:15:15 of dimethylamine is measured formaldehyde solution (being formalin) 102 mL and dimethylamine 165 mL, joins in the mixture C that step 6) obtains 40 ℃ simultaneously, stir, insulation 2h regulates pH=7.5 with hydrochloric acid, gets liquid product D; Wherein the concentration of formaldehyde solution (being formalin) is 37wt%;
8) with liquid product D with 60 ℃ of forced air dryings, namely get the water-soluble polyurethane graft starch water conditioner of solid.
The flocculating effect experiment:
1) gets the 0.5g wilkinite, add and be equipped with in the tool plug graduated measuring glass cylinder of 100 mL water, be made into the bentonite suspension of 0.5wt% concentration.Totally 5 parts, number 1-5 number, wherein be contrast No. 1;
2) accurately take by weighing 0.500 mg water-soluble polyurethane graft starch water conditioner (product), totally 4 parts;
3) in the 2-5 bentonite suspension, add step 2) ready water conditioner (contrast does not add), begin immediately to stir, the 1-5 churning time is respectively 4,1,2,3,4min, and guarantees that stirring stops simultaneously.
4) after stirring finishes, leave standstill, every interval certain hour is observed the sedimentation situation of solution in the graduated cylinder, and takes pictures;
5) compare churning time to the influence of water conditioner effect.
Four kinds of churning time are little to the flocculating effect influence of water conditioner, but time of repose is influential.The 2-5 graduated cylinder all shows as: significantly flocculation interface appears in the time of repose of 4min, and clarified liq volume 81-82mL when 8min, after this prolongation clarification volume change in time is little, and 40min reaches the clarification volume of 82mL.And No. 1 reach the clarification volume that 80 mL just appear in 40min to impinging upon, and mainly is the result of natural subsidence.
The result shows: water-soluble polyurethane graft starch water conditioner has flocculating effect preferably.
Embodiment 3:
A kind of preparation method of water-soluble polyurethane graft starch water conditioner, it comprises the steps:
1) by starch: the weight ratio of water=1:9 takes by weighing starch 10g, measures water 90mL(distilled water), and water and starch stirred, the mixture of starch and water obtained;
2) be warming up to the mixture (insulation 10min obtains starch paste) of 90 ℃ of pasted starches and water, and add the NaOH solution adjusting pH to 11 that concentration is 10wt%, the starch paste of adjusted good pH;
3) by urea: the mol ratio of starch=1:1 takes by weighing urea 4.07g, joins step 2) in regulate in the starch paste of pH, stir, be warming up to 97 ℃, insulation 2h transfers pH to 5.4 with hydrochloric acid, gets mixture A; The concentration of described hydrochloric acid is 10-30wt%;
4) according to starch: the mol ratio of formaldehyde solution: urea=1:7.5:7.5 is measured formaldehyde solution 51mL, takes by weighing urea 30.7g, and wherein the concentration of formaldehyde solution (being formalin) is 37wt%;
5) transfer the pH to 8 of formaldehyde solution with hydrochloric acid, in formaldehyde solution, add urea then, slowly be warmed up to 95 ℃ (slowly refer to temperature rise rate be 1 ℃/min), insulation 2h gets mixture B; The concentration of described hydrochloric acid is 10-30wt%;
6) mixture A is after stirring and being warming up to 90 ℃, and mixture B slowly is added drop-wise among the mixture A and (drips in the 30min), and keeps 90 ℃ of temperature, reacts 60min again, is cooled to 40 ℃, gets mixture C;
7) according to starch: formaldehyde solution: the ratio of the mol ratio=1:7.5:7.5 of dimethylamine is measured formaldehyde solution 51mL and dimethylamine 82.5mL, joins in the mixture C that step 6) obtains 40 ℃ simultaneously, stir, insulation 2h regulates pH=7.5 with hydrochloric acid (HCl), gets liquid product D; Wherein the concentration of formaldehyde solution (being formalin) is 37wt%;
8) with liquid product D with 60 ℃ of forced air dryings, namely get the water-soluble polyurethane graft starch water conditioner of solid.
The flocculating effect experiment:
1) gets the 0.5g wilkinite, add and be equipped with in the tool plug graduated measuring glass cylinder of 100 mL water, be made into the bentonite suspension of 0.5wt% concentration.Totally 5 parts, number 1-5 number, wherein be contrast No. 1;
2) accurately take by weighing 0.500 mg water-soluble polyurethane graft starch water conditioner (product), totally 4 parts;
3) in the 2-5 bentonite suspension, add step 2) ready water conditioner (contrast does not add), begin immediately to stir, the 1-5 churning time is respectively 4,1,2,3,4min, and guarantees that stirring stops simultaneously.
4) after stirring finishes, leave standstill, every interval certain hour is observed the sedimentation situation of solution in the graduated cylinder, and takes pictures;
5) compare churning time to the influence of water conditioner effect.
Four kinds of churning time are little to the flocculating effect influence of water conditioner, but time of repose is influential.The 2-5 graduated cylinder all shows as: occur significantly flocculation interface in the time of repose of 1min, the clarified liq volume has reached 82-85mL when 3min, and after this prolongation clarification volume change in time is little.And No. 1 reach the clarification volume that 80 mL just appear in 40min to impinging upon, and mainly is the result of natural subsidence.
The result shows: water-soluble polyurethane graft starch water conditioner has flocculating effect preferably.Water-soluble the best of water conditioner.
Claims (6)
1. the preparation method of a water-soluble polyurethane graft starch water conditioner is characterized in that it comprises the steps:
1) by starch: the weight ratio of water=1:9 takes by weighing starch, measures water, and water and starch are stirred, and obtains the mixture of starch and water;
2) be warming up to the mixture of 90 ℃ of pasted starches and water, and add NaOH solution adjusting pH to 10-11, the starch paste of adjusted good pH;
3) by urea: the mol ratio of starch=1:1 takes by weighing urea, joins step 2) in regulate in the starch paste of pH, stir, be warming up to 95-97 ℃, insulation 1-2h transfers pH to 4.8-5.4 with hydrochloric acid, gets mixture A;
4) according to starch: the mol ratio of formaldehyde solution: urea=1:1:1-1:15:15 is measured formaldehyde solution, takes by weighing urea;
5) with the pH to 6-8 of hydrochloric acid accent formaldehyde solution, add urea then in formaldehyde solution, be warmed up to 90-95 ℃, insulation 2h gets mixture B;
6) mixture B is splashed among the mixture A, stir, and keep 90 ℃ of temperature, drip off afterreaction 40-60min, be cooled to 40 ℃, get mixture C;
7) according to starch: formaldehyde solution: the ratio of the mol ratio=1:1:1-1:15:15 of dimethylamine is measured formaldehyde solution and dimethylamine, joins in the mixture C that step 6) obtains 40 ℃ simultaneously, stir, insulation 2h regulates pH=6.5-7.5 with hydrochloric acid, gets liquid product D;
8) with liquid product D drying, namely get the water-soluble polyurethane graft starch water conditioner of solid.
2. the preparation method of a kind of water-soluble polyurethane graft starch water conditioner according to claim 1, it is characterized in that: the concentration of described NaOH solution is 10-30wt%.
3. the preparation method of a kind of water-soluble polyurethane graft starch water conditioner according to claim 1, it is characterized in that: the concentration of described hydrochloric acid is 10-30wt%.
4. the preparation method of a kind of water-soluble polyurethane graft starch water conditioner according to claim 1, it is characterized in that: the concentration of described formaldehyde solution is the 37wt% formalin.
5. the preparation method of a kind of water-soluble polyurethane graft starch water conditioner according to claim 1 is characterized in that: in the step 4), according to starch: the mol ratio of formaldehyde solution: urea=1:7.5:7.5 is measured formaldehyde solution, takes by weighing urea.
6. the preparation method of a kind of water-soluble polyurethane graft starch water conditioner according to claim 1 is characterized in that: in the step 7), according to starch: formaldehyde solution: the ratio of the mol ratio=1:7.5:7.5 of dimethylamine is measured formaldehyde solution and dimethylamine.
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| CN102225801A (en) * | 2011-04-19 | 2011-10-26 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of cationized carbamate starch water treatment agent |
| CN102351341A (en) * | 2011-07-06 | 2012-02-15 | 武汉理工大学 | Preparation and application of paint waste water treatment agents |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102225801A (en) * | 2011-04-19 | 2011-10-26 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of cationized carbamate starch water treatment agent |
| CN102351341A (en) * | 2011-07-06 | 2012-02-15 | 武汉理工大学 | Preparation and application of paint waste water treatment agents |
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