CN102351993B - Preparation method for flocculant starch of grafted acryl oxyethyl trimethyl ammonium chloride - Google Patents
Preparation method for flocculant starch of grafted acryl oxyethyl trimethyl ammonium chloride Download PDFInfo
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- CN102351993B CN102351993B CN 201110194782 CN201110194782A CN102351993B CN 102351993 B CN102351993 B CN 102351993B CN 201110194782 CN201110194782 CN 201110194782 CN 201110194782 A CN201110194782 A CN 201110194782A CN 102351993 B CN102351993 B CN 102351993B
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Abstract
The invention relates to a preparation method for flocculant starch used for waste water treatment. A preparation method for flocculant starch of grafted acryl oxyethyl trimethyl ammonium chloride is characterized by comprising the following steps of: 1) high-energy radiation: feeding the starch into a 60Co-gamma ray radiation field under the radiation condition of aerobic radiation at the radiation dosage being 4 to 10Kgy to obtain pre-radiation starch; 2) spraying stirring: selecting the pre-radiation starch and acryl oxyethyl trimethyl ammonium chloride according to the principle that the addition of the acryl oxyethyl trimethyl ammonium chloride is 25 percent to 50 percent of the mass of the pre-radiation starch and obtaining a mixture through carrying out spraying stirring on the pre-radiation starch and the acryl oxyethyl trimethyl ammonium chloride; and 3) grafting reaction in a microwave filed: placing the mixture into a microwave field, carrying out intermittent microwave treatment for 70s to 3min to obtain grafted starch, crushing the grafted starch and obtaining the flocculant starch of the grafted acryl oxyethyl trimethyl ammonium chloride. The flocculant starch prepared by the method has good flocculation effect and low production cost, and the method has a simple process.
Description
Technical field
The present invention relates to a kind of preparation method of the flocculation starch for wastewater treatment.
Background technology
The pollution of water surrounding is one of very outstanding environmental threat of present China.Wastewater treatment is an important integral part of present environmental improvement.The graft starch flocculation agent is the graft copolymer of starch and monomer, has that flocculating effect is good, an advantage such as degradable and raw material cheapness, is the focus of current research.
The relevant patent research of grafting quaternary ammonium salt monomer on the starch.Chinese patent (200610166835.X) is raw material with starch, 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride or N-(2,3-epoxy chloropropionate base) trimethyl ammonium chloride is made cationic etherifying agent, under sodium hydroxide/catalyst promoter composite catalytic system katalysis, the method that is used in is synthesized high degree of substitution quaternary ammonium cationic starch flocculating agent, can be widely used in wastewater treatment and the sludge dewatering of industries such as papermaking, printing and dyeing, process hides, petrochemical complex; Chinese patent (200710055247.3) is main raw material with the W-Gum, adopt cerous sulfate to make initiator, be that cationic monomer carries out modification and makes starch and cation mono precursor copolymer with ammonium chloride and acetic anhydride multipolymer, be applicable to the processing of the higher sanitary sewage of silt content, trade effluent, backwashing wastewater, various sludge from sedimentation tank.But do not relate to irradiation or microwave treatment, and grafted monomer difference.
The relevant patent research of the multiple monomer of grafting on the starch.Chinese patent (200510059924.X), this invention is raw material with a kind of in W-Gum, the carboxymethyl starch, 2 kinds in acrylamide, vinylformic acid, the dimethyl diallyl ammonium chloride is monomer, ammonium persulphate/reductive agent is composite initiator, with solution or reversed emulsion polymerization, carry out terpolymer, get flocculation agent ZMS1; Perhaps, ZMS1 carries out Mannich reaction with formaldehyde and dimethylamine again, gets flocculation agent ZMS2.The purposes of flocculation agent is to handle oily(waste)water, dyeing and printing sewage, water scavengine agent and sterilant, sludge dehydrating agent and heavy metal scavenging agent.Chinese patent (200910016228.9), this invention is base material with starch, adopting chain alkyl allyl dimethyl ammonium chloride and acrylamide is monomer, be reaction medium with water, under the composite initiator effect, make a kind of efficient starch graft copolymer by processing steps such as slurrying, monomer preparation, deoxidation, initiation, reactions, industry such as can be widely used in oil, dehydrating municipal sludge, papermaking, butcher.
Reported and adopted chemical method or multi-component copolymer to prepare the flocculation starch of grafting quaternary ammonium salt monomer in the patent mostly, yet there are no
60The Co-gamma-rays prepares irradiated starch, and then with gained irradiated starch and DAC grafting, patent and the bibliographical information of the flocculation starch of preparation grafting DAC.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, the flocculating effect of the flocculation starch of this method preparation is good, and this method technology is simple.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac is characterized in that it comprises the steps:
1) high-energy irradiation: starch is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (namely carrying out irradiation under atmospheric environment or under the condition of aerobic), and radiation dose is 4-10KGy, make described starch produce free radical, obtain pre-irradiation starch;
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is the 25%-50% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, and batch microwave is handled 70s-3min, obtains graft starch, and graft starch is pulverized, and obtains the flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac.
Described starch is W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch or sweet potato starch; Described DAC is acrylyl oxy-ethyl-trimethyl salmiac.
Described
60Co-gamma-rays radiation field is 400,000 Curie's industrial dynamic source of radiation (industrial dynamic radiation devices) for the loading of source amount.
It is 20s that described batch microwave is treated to microwave treatment time, and the intermittent time is 5-15s.
The power of described microwave treatment is 500～1000W, and frequency is 900-2500MHz.
Described atmospheric environment refers to the air conditions of normal temperature and pressure, because there is oxygen, is again that aerobic is handled, and can be described as aerobic irradiation.
The flocculation starch of grafting DAC of the present invention, the percentage of grafting of this flocculation starch is 19%-40%, is a kind of flocculation starch that has cationic quaternary ammonium group.
Beneficial effect of the present invention: realize that fully it has also reduced production cost flocculating effect the time efficiently, has reduced pollution.No matter be production process itself, or last handling process all is energy-conservation and environmental protection.
Principal feature is: 1. the present invention uses the method that high-energy ray irradiation causes, and will effectively be grafted on the starch by grafts, and this technology efficiency of initiation height, aftertreatment are simple, and flocculating effect is good, and characteristics such as the flocculation after product is easily separated; 2. the semidry process that adopts spraying to stir has advantages such as energy-conservation, efficient, water saving; Advantages such as 3. adopt microwave exposure processing, production process obviously shortens, and process energy consumption is low, and it is simple to have technology, and investment goods is few; 4. the raw material that uses among the present invention all has good thermostability, and nontoxic, non-volatility is conducive to environment protection and operator ' s health, and the production efficiency height meets the requirement of green production.
Flocculation starch of the present invention is applicable to waste water from dyestuff, petrochemical wastewater, paper waste field of purification.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention, should be understood that these examples only are used for explanation the present invention and are not used in and limit the scope of the invention.Should be understood that in addition that after the content of having read the present invention's instruction those skilled in the art can do work to the present invention and change or revise, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
In following examples: described
60Co-gamma-rays radiation field is 400,000 Curie's industrial dynamic source of radiation (industrial dynamic radiation devices) for the loading of source amount.
Embodiment 1:
A kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, it comprises the steps:
1) high-energy irradiation: W-Gum is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (namely carrying out irradiation under atmospheric environment), and radiation dose is 6KGy, make described W-Gum produce free radical, obtain pre-irradiation starch (being the pre-irradiation W-Gum);
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is 50% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, make it fully mix, be half-dried attitude, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled, every microwave 20s, 5s intermittently, microwave is 7 times altogether, play desiccation when making active group on starch free radical and the DAC carry out graft reaction, the graft starch of generation after crushed, a rate that obtains is the flocculation starch of 39.5% grafted propylene acyl-oxygen ethyl-trimethyl salmiac.
This flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 18s, gets transmittance that supernatant liquid records behind the 15min greater than 82%.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 2:
A kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, it comprises the steps:
1) high-energy irradiation: tapioca (flour) is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (namely under atmospheric environment), and radiation dose is 4KGy, make described tapioca (flour) produce free radical, obtain pre-irradiation starch (being the pre-irradiation tapioca (flour));
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is 30% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, make it fully mix, be half-dried attitude, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled, every microwave 20s, 5s intermittently, microwave is 6 times altogether, play desiccation when making active group on starch free radical and the DAC carry out graft reaction, the graft starch of generation after crushed, obtaining percentage of grafting is 32.4% grafted propylene acyl-oxygen ethyl-trimethyl salmiac flocculation starch.
This flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 20s, gets transmittance that supernatant liquid records behind the 15min greater than 80%.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 3:
A kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, it comprises the steps:
1) high-energy irradiation: sorghum starch is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (the volume oxygen level is 30% nitrogen oxygen mixed gas), and radiation dose is 4KGy, make described sorghum starch produce free radical, obtain pre-irradiation starch;
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is 25% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, make it fully mix, be half-dried attitude, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled, every microwave 20s, 5s intermittently, microwave 5 times, play desiccation when making active group on starch free radical and the DAC carry out graft reaction, the graft starch of generation obtains percentage of grafting and is 28.1% grafted propylene acyl-oxygen ethyl-trimethyl salmiac flocculation starch after crushed.
This flocculation starch is used for the processing of sanitary wastewater hexavalent chromium, and the clearance rate of hexavalent chromium can reach 95% under neutrallty condition.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 4:
A kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, it comprises the steps:
1) high-energy irradiation: sweet potato starch is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (namely carrying out irradiation under atmospheric environment), and radiation dose is 6KGy, make described sweet potato starch produce free radical, obtain pre-irradiation starch;
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is 35% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, make it fully mix, be half-dried attitude, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled, every microwave 20s, 5s intermittently, microwave 5 times, play desiccation when making active group on starch free radical and the DAC carry out graft reaction, the graft starch of generation obtains percentage of grafting and is 33.2% grafted propylene acyl-oxygen ethyl-trimethyl salmiac flocculation starch after crushed.
This flocculation starch is used for the processing of kaolin suspension liquid, and settling velocity is less than 10s, gets transmittance that supernatant liquid records behind the 15min greater than 90%.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 5:
A kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, it comprises the steps:
1) high-energy irradiation: wheat starch is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (namely carrying out irradiation under atmospheric environment), and radiation dose is 10KGy, make described wheat starch produce free radical, obtain pre-irradiation starch;
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is 25% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled 70s, and (microwave treatment time is 20s, intermittent time is 5s, microwave is 3 times altogether), play desiccation when making active group on starch free radical and the DAC carry out graft reaction, the graft starch that generates obtains percentage of grafting and is 42% grafted propylene acyl-oxygen ethyl-trimethyl salmiac flocculation starch after crushed.
This flocculation starch is used for the processing of acid blue dye waste water, and settling velocity is less than 16s, gets transmittance that supernatant liquid records behind the 15min greater than 80%.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 6:
A kind of preparation method of flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac, it comprises the steps:
1) high-energy irradiation: Starch rice is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation (namely carrying out irradiation under atmospheric environment), and radiation dose is 8KGy, make described Starch rice produce free radical, obtain pre-irradiation starch;
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac (DAC) is 40% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC); Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac (DAC) are stirred through spraying, make it fully mix, be half-dried attitude, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled 3min, and (microwave treatment time is 20s, intermittent time is 12s, microwave is 6 times altogether), play desiccation when making active group on starch free radical and the DAC carry out graft reaction, the graft starch that generates obtains percentage of grafting and is 40% grafted propylene acyl-oxygen ethyl-trimethyl salmiac flocculation starch after crushed.
This flocculation starch is used for the processing of paper waste cadmium ion, and the clearance rate of cadmium ion can reach 98% under neutrallty condition.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 7:
Substantially the same manner as Example 1, difference is: W-Gum substitutes with yam starch.
Resulting flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 18s, gets transmittance that supernatant liquid records behind the 15min greater than 82%.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Embodiment 8:
Substantially the same manner as Example 1, difference is: W-Gum substitutes with pueraria starch.
Resulting flocculation starch is used for the processing of acid red dye waste water, and settling velocity is less than 18s, gets transmittance that supernatant liquid records behind the 15min greater than 82%.The flocculating effect that the flocculation starch that this embodiment prepares is described is good.
Each raw material that the present invention is cited and the bound value of each raw material, and the bound value of each processing parameter can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (3)
1. the preparation method of the flocculation starch of a grafted propylene acyl-oxygen ethyl-trimethyl salmiac is characterized in that it comprises the steps:
1) high-energy irradiation: starch is sent into
60Co-gamma-rays radiation field, radiation parameter are aerobic irradiation, and radiation dose is 4-10KGy, make described starch produce free radical, obtain pre-irradiation starch;
2) spraying is stirred: the add-on by acrylyl oxy-ethyl-trimethyl salmiac is the 25%-50% of pre-irradiation starch quality, chooses pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac; Pre-irradiation starch and acrylyl oxy-ethyl-trimethyl salmiac are stirred through spraying, obtain mixture;
3) carry out graft reaction in the microwave field: mixture is placed microwave field, batch microwave is handled 70s-3min, it is 20s that described batch microwave is treated to microwave treatment time, intermittent time is 5-15s, obtain graft starch, graft starch is pulverized, and obtains the flocculation starch of grafted propylene acyl-oxygen ethyl-trimethyl salmiac.
2. the preparation method of the flocculation starch of a kind of grafted propylene acyl-oxygen ethyl-trimethyl salmiac according to claim 1, it is characterized in that: described starch is W-Gum, wheat starch, sorghum starch, Starch rice, yam starch, tapioca (flour), pueraria starch or sweet potato starch.
3. the preparation method of the flocculation starch of a kind of grafted propylene acyl-oxygen ethyl-trimethyl salmiac according to claim 1 is characterized in that: described
60Co-gamma-rays radiation field is 400,000 Curie's industrial dynamic source of radiation for the loading of source amount.
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| CN104804137A (en) * | 2015-01-31 | 2015-07-29 | 武汉纺织大学 | Preparation method of water-soluble cationic grafted starch |
| CN107151291A (en) * | 2017-07-11 | 2017-09-12 | 武汉纺织大学 | A kind of technique of utilization dry production graft starch |
| CN108559089A (en) * | 2018-04-18 | 2018-09-21 | 西安石油大学 | A kind of preparation method of waste liquid of drilling separation of solid and liquid degradable macromolecule gel breaker |
| CN108929024A (en) * | 2018-08-31 | 2018-12-04 | 昆明理工大学 | A kind of sludge reduction and innoxious method |
| CN109880010A (en) * | 2019-03-27 | 2019-06-14 | 湖北顶新环保生物质材料有限公司 | A kind of starch-based composite flocculant and its preparation method and application |
| CN109912745A (en) * | 2019-03-27 | 2019-06-21 | 湖北顶新环保生物质材料有限公司 | A kind of starch-based composite flocculant and its preparation method and application |
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| CN101177457A (en) * | 2007-10-30 | 2008-05-14 | 广州辐照技术研究开发中心 | Method for preparing dicyandiamide-formaldehyde resin branched starch ether by employing radiation initiation |
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| "60Coγ射线预辐照制备淀粉-丙烯酰胺接枝物";包华影等;《辐射研究与辐射工艺学报》;20001130;第18卷(第4期);263-267 * |
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