CN103992413A - Synthetic method of cross-linked acetate cation double-modified starch printing and dyeing wastewater treating agent - Google Patents
Synthetic method of cross-linked acetate cation double-modified starch printing and dyeing wastewater treating agent Download PDFInfo
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Abstract
The invention relates to a synthetic method of a cross-linked acetate cation double-modified starch printing and dyeing wastewater treating agent. According to the method, esterification and crosslinking between corn starch and an anion esterification cross-linking agent is firstly carried out; and then, a cation etherification reagent 3-chloro-2hydroxypropyl trimethylammonium chloride is used to carry out a reaction so as to obtain the double-modified starch printing and dyeing wastewater treating agent, wherein the anion esterification cross-linking agent is mixed anhydride prepared from acetic anhydride and adipic acid. Cationic groups of the acetate cation double-modified starch prepared by the method are completely ionized in water, and positive charge has high density and can catch negatively-charged suspended particles; and anionic groups also can promote sedimentation of inorganic suspensions and play a role in bridging and coagulation enhancement. The two groups have different adsorption and flocculation properties, supplementing each other. Thus, an ideal flocculation and decolouring effect is achieved.
Description
Technical field
The synthetic method that the present invention relates to the two modified starch treatment of dyeing/printing wastewaters of a kind of crosslinked acetic ester positively charged ion, belongs to chemical technology field.
Background technology
Along with the fast development of China's economy, problem of environmental pollution is day by day serious, the focus that wherein atmosphere is administered, water conservation is just becoming people's concern.Water pollutes and comprises that trade effluent and sanitary wastewater pollute two kinds, and in trade effluent, the waste water of textile industry, Pulp industry occupies sizable ratio, and dyeing year, waste discharge was about 3,000,000,000 tons of left and right.Dyeing waste water belongs to the organic waste water of high density, poisonous and harmful, difficult degradation, contain residual dye, dyeing auxiliary, soda acid and some heavy metal, wherein residual dye and auxiliary agent have formed organic main component in waste water, and make waste water with special color, therefore, how to make decolorizing printing and dyeing waste water become current pending major issue, the research of decoloring method also becomes the important topic for the treatment of of dyeing wastewater.
For a long time, Coagulation Method has that investment cost is low, equipment takes up an area less, processing capacity is large, percent of decolourization advantages of higher, is still now the method for wastewater treatment that the middle-size and small-size printing and dyeing enterprise of China generally adopts.Selecting efficient flocculation agent and effective coagulation decoloration technique is the key of this technology, the main flocculation agent of current decolorizing printing and dyeing waste water taking polyacrylamide PAM as main synthetic polymer, but the toxicity problem of synthetic polymeric flocculant, difficult degradation problem receive publicity day by day, and the superiority of natural macromolecule flocculating agent is also favored gradually.Since the 90's of 20th century, in world wide, there is the new interest to natural macromolecule flocculating agent research and development, the research fields such as starch derivative, vegetable jelly modified water treatment agent, microbial flocculant and chitin derivativ all become new study hotspot gradually, the water conditioner that natural high moleculer eompound modification obtains, show in this respect incomparable advantage, it is nontoxic to environment, and process residue be easily biodegradable, can not cause secondary pollution to environment.
Summary of the invention
The object of the present invention is to provide the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of a kind of crosslinked acetic ester positively charged ion, the two modified starch treatment of dyeing wastewater of crosslinked acetic ester positively charged ion that the method makes, in flocculation, there is stronger decoloring ability, in the time for the treatment of of dyeing and printing, have more flco large, separate soon, the advantage such as higher loading capacity.
The object of the present invention is achieved like this: the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of a kind of crosslinked acetic ester positively charged ion, first W-Gum is carried out to esterification and crosslinking with negatively charged ion esterification linking agent (aceticanhydride, hexanodioic acid mixed anhydride), then react with chloro-2 hydroxypropyl-trimethyl ammonium chlorides of positively charged ion etherifying reagent 3-the two modified starch treatment of dyeing/printing wastewaters that obtain.
Described negatively charged ion esterification linking agent is mixed by diacetyl oxide and hexanodioic acid mixed anhydride.
The preferred version of the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of a kind of crosslinked acetic ester positively charged ion is, take a certain amount of W-Gum, add deionized water, be warming up to 40 DEG C～50 DEG C, adjust in the scope of pH value to 7～9 with NaOH solution, add self-control esterification and crosslinking agent (diacetyl oxide and hexanodioic acid mixed anhydride), insulation reaction 1～3 hour, product is poured in deionized water, leave standstill 3 hours, remove supernatant liquid, washing is to neutral, dehydration, puts into baking oven and at 55 DEG C, dries and must be cross-linked acetate starch in 20 hours;
Then take crosslinked acetate starch, add deionized water, taking NaOH solution regulation system pH value as 9～11, heating makes reaction system be warming up to 40 DEG C～50 DEG C, adds while stirring the mixed solution of the chloro-2 hydroxypropyl-trimethyl ammonium chloride etherifying agents of 3-and NaOH, reaction times 4-10h, reaction finishes the rare HCl of rear use and is adjusted to pH value and equals 7, filter, with ethanol/water mixing solutions repetitive scrubbing, dry, grinding, and sieve with 100 order/25.4 mm sub-sieves.
Described esterification and crosslinking agent: by diacetyl oxide and hexanodioic acid in mass ratio the ratio of 10～20:1 mix, after 20～35 DEG C of degree stir 10～20min, leave standstill and can obtain water white esterification and crosslinking agent mixed anhydride with magnetic stirring apparatus.
NaOH strength of solution is 5～20%.
Starch, deionized water bath raio equal 200～1000g/L.
The mass ratio that feeds intake of esterification and crosslinking reagent mixed anhydride and W-Gum is: 0.1～0.4:100
The mass ratio that feeds intake of cationic etherifying agent and crosslinked acetate starch is: 5～20:100
Preferred version is: take a certain amount of W-Gum, add deionized water, bath raio 650g/L, be warming up to 45 DEG C, adjust pH value to 8 left and right with 10%NaOH solution, drip the self-control esterification and crosslinking agent (diacetyl oxide and hexanodioic acid mixed anhydride) of starch quality 0.2%, when reaction, keeping pH value is 8, insulation reaction 1.5h, pours product in doubling dose ionized water into, leaves standstill 3 hours, remove supernatant liquid, washing is to neutral, and dehydration is put into baking oven and at 55 DEG C, dried and must be cross-linked acetate starch in 20 hours.
Take crosslinked acetate starch, add deionized water; bath raio 650g/L, taking 10%NaOH solution regulation system pH value as 11, heating makes reaction system be warming up to 45 DEG C; add while stirring the mixed solution of the chloro-2 hydroxypropyl-trimethyl ammonium chloride etherifying agents of 3-and NaOH; reaction times 6h, and reaction finishes the rare HCl of rear use, and to be adjusted to pH value be neutral, filters; with ethanol/water (1:1) mixing solutions repetitive scrubbing, be dried, grinding, and sieve with 100 order/25.4 mm sub-sieves.
The invention has the beneficial effects as follows:
1, the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, when waste water from dyestuff for cotton (substantive dyestuff, reactive dyestuffs, bipseudoindoxyl dye, dispersed dye etc.) is carried out to flocculation decoloration, usage quantity is that 0.2 g/L color degree of dyeing waste water clearance can reach more than 90%, and when usage quantity is 0.4 g/L, color degree of dyeing waste water clearance can reach more than 98%.
2, the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion from flocculation decoloration water technology relatively, what enterprise adopted now is PAM flocculation and clorox decolouring recombining process, and amphoteric starch treatment of dyeing/printing wastewaters treatment process prepared by this law is simple; And PAM processing residue may produce micro-malicious carcinogens, after entered environment, cause secondary pollution, the amphoteric starch water conditioner that modification obtains as natural high moleculer eompound, show in this respect incomparable advantage, it is nontoxic to environment, and process residue and be easily biodegradable, can not cause secondary pollution to environment.
Embodiment
Embodiment 1:
The present invention relates to the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, and described method comprises following processing step:
Take a certain amount of W-Gum, add deionized water, bath raio 650g/L, be warming up to 45 DEG C, adjust pH value to 8 left and right with 10%NaOH solution, (diacetyl oxide reacts the mixed anhydride made from hexanodioic acid in the self-control esterification and crosslinking agent of dropping starch quality 0.15%, by diacetyl oxide and hexanodioic acid in mass ratio the ratio of 10:1 mix, can obtain water white esterification and crosslinking agent mixed anhydride with magnetic stirring apparatus is standing after 20 DEG C of degree stir 15min), when reaction, keeping pH value is 8, insulation reaction 1h, product is poured in doubling dose ionized water, leave standstill 3 hours, remove supernatant liquid, washing is to neutral, dehydration, put into baking oven dries and must be cross-linked acetate starch in 20 hours at 55 DEG C.
Take crosslinked acetate starch, add deionized water; bath raio 650g/L, crosslinked acetate starch and etherifying agent (chloro-2 hydroxypropyl-trimethyl ammonium chlorides of 3-) mass ratio are 10:1,40 DEG C of temperature of reaction; pH value is 11; 2.5 hours reaction times, and reaction finishes the rare HCl of rear use and is adjusted to extremely neutrality of pH value, filters; with ethanol/water (1:1) mixing solutions repetitive scrubbing, dry, grinding, and sieve with 100 order/25.4 mm sub-sieves.Make the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, Anion substituting degree is 0.0739, and positively charged ion substitution value is 0.0085.
Embodiment 2:
The present invention relates to the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, and described method comprises following processing step
Take a certain amount of W-Gum, add deionized water, bath raio 650g/L, be warming up to 45 DEG C, with 10%NaOH solution adjust pH to 9 left and right, (diacetyl oxide reacts the mixed anhydride made from hexanodioic acid in the self-control esterification and crosslinking agent of dropping starch quality 0.20%, by diacetyl oxide and hexanodioic acid in mass ratio the ratio of 10:1 mix, can obtain water white esterification and crosslinking agent mixed anhydride with magnetic stirring apparatus is standing after 20 DEG C of degree stir 15min), when reaction, keeping pH value is 9, insulation reaction 1.5h, product is poured in doubling dose ionized water, leave standstill 3 hours, remove supernatant liquid, washing is to neutral, dehydration, put into baking oven dries and must be cross-linked acetate starch in 20 hours at 55 DEG C.
Take crosslinked acetate starch, add deionized water; bath raio 650g/L, crosslinked acetate starch and etherifying agent (chloro-2 hydroxypropyl-trimethyl ammonium chlorides of 3-) mass ratio are 8:1,45 DEG C of temperature of reaction; pH value is 11; 6 hours reaction times, and reaction finishes the rare HCl of rear use and is adjusted to extremely neutrality of pH value, filters; with ethanol/water (1:1) mixing solutions repetitive scrubbing, dry, grinding, and sieve with 100 order/25.4 mm sub-sieves.Make the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, Anion substituting degree is 0.0745, and positively charged ion substitution value is 0.0131.
Embodiment 3:
Take a certain amount of W-Gum, add deionized water, bath raio 650g/L, be warming up to 50 DEG C, with 10%NaOH solution adjust pH to 8 left and right, (diacetyl oxide reacts the mixed anhydride made from hexanodioic acid in the self-control esterification and crosslinking agent of dropping starch quality 0.15%, by diacetyl oxide and hexanodioic acid in mass ratio the ratio of 10:1 mix, can obtain water white esterification and crosslinking agent mixed anhydride with magnetic stirring apparatus is standing after 20 DEG C of degree stir 15min), when reaction, keeping pH value is 8, insulation reaction 2h, product is poured in doubling dose ionized water, leave standstill 3 hours, remove supernatant liquid, washing is to neutral, dehydration, put into baking oven dries and must be cross-linked acetate starch in 20 hours at 55 DEG C.
Take crosslinked acetate starch, add deionized water; bath raio 650g/L, crosslinked acetate starch and etherifying agent (chloro-2 hydroxypropyl-trimethyl ammonium chlorides of 3-) mass ratio are 5:1,45 DEG C of temperature of reaction; pH value of reaction system is 11; 6 hours reaction times, and reaction finishes the rare HCl of rear use and is adjusted to extremely neutrality of pH value, filters; with ethanol/water (1:1) mixing solutions repetitive scrubbing, dry, grinding, and sieve with 100 order/25.4 mm sub-sieves.Make the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, Anion substituting degree is 0.0705, and positively charged ion substitution value is 0.0220.
Get respectively crosslinked acetate starch (Anion substituting degree 0.0745), cationic starch (the chloro-2 hydroxypropyl-trimethyl ammonium chloride positively charged ion substitution values 0.0130 of 3-), crosslinked acetic ester amphoteric starch (embodiment 1: Anion substituting degree is 0.0739, positively charged ion substitution value is 0.0085; Embodiment 2: Anion substituting degree is 0.0745, positively charged ion substitution value is 0.0131; Embodiment 3: Anion substituting degree is 0.0705, positively charged ion substitution value is 0.0220.) carrying out dyeing waste water (containing matching stain, reactive dyestuffs, substantive dyestuff, bipseudoindoxyl dye) Decolorant Test, decolorizing effect sees the following form
Table all kinds starch water conditioner color degree of dyeing waste water clearance contrast table
As can be seen from the above table, the crosslinked acetate starch of identical Anion substituting degree is compared with crosslinked acetate starch amphoteric starch, reinforced while being all 0.2g/L, color degree of dyeing waste water clearance is 90.64% by 28.91% rising, crosslinked acetate starch amphoteric starch effect is better than crosslinked acetic ester anionic starch greatly, the cationic starch of identical positively charged ion substitution value and crosslinked acetate starch amphoteric starch, reinforced while being all 0.2g/L, color degree of dyeing waste water clearance is 90.64% by 50.13% rising, crosslinked acetate starch amphoteric starch decolorizing effect is significantly better than cationic ion starch.While reaching 0.4g/L when feeding in raw material, the color degree of dyeing waste water clearance of crosslinked acetate starch amphoteric starch can reach 98.83%.
This is because contain the positively charged ion that is that the dyestuffs such as matching stain, reactive dyestuffs, substantive dyestuff, bipseudoindoxyl dye have in water in dyeing waste water, and what have is negatively charged ion in water, and because amphoteric starch is because having the Pollution System that is applicable to yin, yang ion coexist.Amphoteric starch flocculation agent cation group is ionization completely in water, positive charge density is high, the suspended particles of energy pull-in range negative charge, and anionic group can promote the sedimentation of inorganic suspended substance, plaing a part to build bridge, it is solidifying to help, two kinds of groups are brought into play different adsorption-flocculation performances, complement each other, and obtain desirable flocculating decoloring effect.
Claims (6)
1. the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of crosslinked acetic ester positively charged ion, it is characterized in that: first first W-Gum is carried out to esterification and crosslinking with negatively charged ion esterification linking agent, then react with chloro-2 hydroxypropyl-trimethyl ammonium chlorides of positively charged ion etherifying reagent 3-the two modified starch treatment of dyeing/printing wastewaters that obtain; Described negatively charged ion esterification linking agent is the mixed anhydride that diacetyl oxide and hexanodioic acid are made.
2. the synthetic method that is cross-linked according to claim 1 the two modified starch treatment of dyeing/printing wastewaters of acetic ester positively charged ion, is characterized in that: in described negatively charged ion esterification linking agent, diacetyl oxide and hexanodioic acid mass ratio are 10～20:1.
3. the synthetic method that is cross-linked according to claim 1 the two modified starch treatment of dyeing/printing wastewaters of acetic ester positively charged ion, is characterized in that: described preparation process comprises:
Take a certain amount of W-Gum, add deionized water, be warming up to 40 DEG C～50 DEG C, in the scope of NaOH solution adjust pH to 7～9, add negatively charged ion esterification linking agent, insulation reaction 1～3 hour, pours product in deionized water into, leaves standstill, remove supernatant liquid, washing is to neutral, and dehydration, puts into oven for drying and must be cross-linked acetate starch;
Take crosslinked acetate starch, add deionized water, taking NaOH solution regulation system pH value as 9～11, heating makes reaction system be warming up to 40 DEG C～50 DEG C, adds while stirring the mixed solution of the chloro-2 hydroxypropyl-trimethyl ammonium chloride etherifying agents of 3-and NaOH, reaction times 4-10h, react and finish the rare HCl adjustment of rear use pH value to neutral relatively good, filter, use ethanol/water mixing solutions repetitive scrubbing, be dried, grind, and sieve with 100 order/25.4 mm sub-sieves, obtain finished product.
4. according to the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of the described crosslinked acetic ester positively charged ion of one of claim 1-3, it is characterized in that: described negatively charged ion esterification linking agent preparation method mixes diacetyl oxide with hexanodioic acid, can obtain water white esterification and crosslinking agent with magnetic stirring apparatus is standing after 20～35 DEG C of degree stir 10～20min.
5. be cross-linked according to claim 3 the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of acetic ester positively charged ion, it is characterized in that: the technique of crosslinked acetate starch esterification and crosslinking is: pH value is 8, W-Gum, deionized water bath raio are 650g/L, the add-on of esterification and crosslinking agent is 0.2% of W-Gum, 45 DEG C of temperature of reaction, the reaction times is 1.5h.
6. be cross-linked according to claim 3 the synthetic method of the two modified starch treatment of dyeing/printing wastewaters of acetic ester positively charged ion, it is characterized in that: the technique of the two modified starch positively charged ion etherificates of crosslinked acetic ester positively charged ion is: pH value is 11, crosslinked acetate starch, deionized water bath raio are 650g/L, the add-on of chloro-2 hydroxypropyl-trimethyl ammonium chlorides of etherifying agent 3-is crosslinked acetate starch 8%, 45 DEG C of temperature of reaction, the reaction times is 6h.
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| CN104356246A (en) * | 2014-09-05 | 2015-02-18 | 北京联合大学 | Cross-linked modified cationic starch flocculant and preparation method thereof |
| CN104437436A (en) * | 2014-12-09 | 2015-03-25 | 鞍钢集团矿业公司 | Magnetite concentrate filter aid and preparation method of solution of magnetite concentrate filter aid |
| CN105776481A (en) * | 2016-03-16 | 2016-07-20 | 江阴职业技术学院 | Xanthate cation dual-modified straw fiber printing and dyeing wastewater treatment agent and preparation method thereof |
| CN110759413A (en) * | 2019-11-01 | 2020-02-07 | 临沂舜驰生态科技有限公司 | Printing and dyeing wastewater treatment agent and treatment method |
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