CN102211804B - Preparation method of starch-based flocculating agent - Google Patents
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Abstract
本发明涉及一种淀粉基絮凝剂的制备方法。一种淀粉基絮凝剂的制备方法,其特征在于包括下列步骤:1)将淀粉置于60Co-γ辐照场中进行辐照,得到预辐照淀粉;2)按接枝单体的加入量为预辐照淀粉质量的50%-100%,按预辐照淀粉与水的质量比为1∶1~1∶3;将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水,开动机器搅拌,得到混合物;3)将搅拌均匀的混合物置于微波炉中间歇微波1~3min,使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;4)将微波后的接枝淀粉在80~140℃条件下烘焙5~10小时,经粉碎,得到淀粉基絮凝剂。该方法具有工艺简单、投资设备少、成本较低,并能获得良好的絮凝效果,且絮凝产物易分离,不会对环境造成二次污染。The invention relates to a preparation method of a starch-based flocculant. A preparation method of a starch-based flocculant, characterized in that it comprises the following steps: 1) placing the starch in a 60 Co-γ irradiation field for irradiation to obtain pre-irradiated starch; 2) adding grafted monomers The amount is 50%-100% of the pre-irradiated starch mass, and the mass ratio of the pre-irradiated starch to water is 1:1 to 1:3; the pre-irradiated starch is placed in the mixer, and the graft monomer is placed In the mixer, add water, start the machine to stir, and obtain the mixture; 3) Put the evenly stirred mixture in the microwave oven for 1-3 minutes to microwave intermittently, so that the starch free radicals react with the active groups on the grafted monomers to form grafted starch; 4) baking the microwaved grafted starch at 80-140° C. for 5-10 hours, and crushing to obtain a starch-based flocculant. The method has the advantages of simple process, less investment equipment, low cost, good flocculation effect, easy separation of flocculation products, and no secondary pollution to the environment.
Description
技术领域 technical field
本发明属于天然高分子絮凝剂技术领域,特别是涉及一种淀粉基絮凝剂的制备方法。The invention belongs to the technical field of natural polymer flocculants, in particular to a preparation method of a starch-based flocculant.
背景技术 Background technique
随着国内经济的快速增长,工业用水量不断增加,工业废水也大量产生,据统计,仅2001年全国工业和城镇生活废水排放总量就为428.4亿吨,其中工业废水排放量200.7亿吨,占废水排放总量的46.7%。2008年全国工业废水排放量为241.7亿吨,其中30%以上的废水未经处理直接排入江河湖海,再生水(污水经净化处理后恢复其使用功能的水)在工业中的利用量也仅相当于取水量的0.4%。工业发展给人们带来经济上的增长和物质上的富足的同时,也给人类赖以生存的不可再生的水资源造成巨大的压力,且未经净化处理的污水的直接排放,对人们的生存环境及生命安全造成极大的危害。在今后的几年供水紧张和污水净化将成为我国乃至世界面临的主要难题之一,因此高效环保的絮凝剂的研究显得尤为重要。With the rapid growth of the domestic economy, industrial water consumption continues to increase, and industrial wastewater is also produced in large quantities. According to statistics, the total discharge of industrial and urban domestic wastewater in the country in 2001 alone was 42.84 billion tons, of which industrial wastewater discharge was 20.07 billion tons. Accounting for 46.7% of the total wastewater discharge. In 2008, the national industrial wastewater discharge amounted to 24.17 billion tons, of which more than 30% of the wastewater was discharged directly into rivers, lakes and seas without treatment. Equivalent to 0.4% of water withdrawal. While industrial development brings economic growth and material abundance to people, it also puts enormous pressure on the non-renewable water resources on which human beings depend, and the direct discharge of unpurified sewage has a negative impact on people's survival. Great harm to the environment and life safety. In the next few years, the shortage of water supply and the purification of sewage will become one of the main problems faced by our country and the world. Therefore, the research on efficient and environmentally friendly flocculants is particularly important.
发明内容 Contents of the invention
本发明的目的在于提供一种淀粉基絮凝剂的制备方法,该方法具有工艺简单、投资设备少、成本较低,并能获得良好的絮凝效果。The purpose of the present invention is to provide a method for preparing a starch-based flocculant, which has the advantages of simple process, less investment in equipment, low cost and good flocculation effect.
为实现上述目的,本发明所采用的技术方案是:一种淀粉基絮凝剂的制备方法,其特征在于包括下列步骤:In order to achieve the above object, the technical solution adopted in the present invention is: a kind of preparation method of starch-based flocculant, it is characterized in that comprising the following steps:
1)将淀粉置于60Co-γ辐照场中,在有氧条件下进行辐照,辐照剂量为4~10KGy,使得淀粉产生自由基,得到预辐照淀粉;1) Put the starch in a 60 Co-γ irradiation field, and irradiate it under aerobic conditions. The irradiation dose is 4-10KGy, so that the starch generates free radicals and obtains the pre-irradiated starch;
2)按接枝单体的加入量为预辐照淀粉质量的50%-100%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水的质量比为1∶1~1∶3,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵(丙烯酰氧乙基三甲基氯化铵为DAC),丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为3∶7~7∶3;2) The addition of grafted monomers is 50%-100% of the pre-irradiated starch quality, select pre-irradiated starch and grafted monomers; the mass ratio of pre-irradiated starch and water is 1: 1 ~ 1 : 3, choose water; Wherein, grafting monomer is acrylamide and acryloyloxyethyltrimethylammonium chloride (acryloyloxyethyltrimethylammonium chloride is DAC), acrylamide and acryloyloxyethyl The mass ratio of trimethyl ammonium chloride is 3: 7~7: 3;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波1~3min(每次微波时间为10~22.5s,间歇5~15s,总共微波4~8次),使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the evenly stirred mixture in a microwave oven for 1-3min intermittently (10-22.5s for each microwave, 5-15s for 5-15s intermittently, 4-8 microwaves in total), so that starch free radicals and grafted monomers The active groups react to generate grafted starch;
4)将微波后的接枝淀粉在80~140℃条件下烘焙5~10小时,经粉碎,得到淀粉基絮凝剂。4) Baking the grafted starch after microwave at 80-140° C. for 5-10 hours, and crushing to obtain a starch-based flocculant.
步骤1)所述的淀粉为玉米淀粉、小麦淀粉、高粱淀粉、大米淀粉、马铃薯淀粉、木薯淀粉、葛根淀粉、甘薯淀粉等中的任意一种。The starch described in step 1) is any one of corn starch, wheat starch, sorghum starch, rice starch, potato starch, tapioca starch, kudzu starch, sweet potato starch and the like.
所述的淀粉含水率为12~16wt%。The moisture content of the starch is 12-16 wt%.
所述丙烯酰胺是一种白色晶体化学物质,是生产水处理用絮凝剂的原料之一。The acrylamide is a white crystalline chemical substance and is one of the raw materials for producing flocculants for water treatment.
所述丙烯酰氧乙基三甲基氯化铵(Aacryloxyethyltrimethyl Ammonium Chloride)(丙烯酰氧乙基三甲基氯化铵为DAC)是一种季胺类阳离子单体,本身带有正电荷,对水中的阴离子有很强的吸附效果。The acryloyloxyethyltrimethylammonium chloride (Aacryloxyethyltrimethyl Ammonium Chloride) (acryloyloxyethyltrimethylammonium chloride is DAC) is a kind of quaternary ammonium cationic monomer, which itself has a positive charge. Anions in water have a strong adsorption effect.
所述60Co-γ辐照场是装源量40万居里的工业用动态辐射装置,是辐射源照射样品的混凝土室。The 60 Co-γ irradiation field is an industrial dynamic radiation device with a source capacity of 400,000 Curies, and it is a concrete chamber where the radiation source irradiates samples.
所述的微波的功率为500~1000W。The power of the microwave is 500-1000W.
本发明的天然高分子絮凝剂适用于染料废水、石化废水、造纸废水净化领域。The natural polymer flocculant of the invention is suitable for the purification fields of dye wastewater, petrochemical wastewater and papermaking wastewater.
本发明的有益效果:1)利用辐射-微波法对天然高分子进行物理改性,制备淀粉基絮凝剂。该方法具有工艺简单、投资设备少、成本较低,并能获得良好的絮凝效果,且絮凝产物易分离,不会对环境造成二次污染。Beneficial effects of the present invention: 1) The starch-based flocculant is prepared by physically modifying natural macromolecules by radiation-microwave method. The method has the advantages of simple process, less investment equipment, low cost, good flocculation effect, easy separation of flocculation products, and no secondary pollution to the environment.
2)本发明中使用的原料均具有良好的热稳定性,无毒、无挥发性,有利于环境保护和操作人员健康,生产效率高,符合绿色生产的要求。2) The raw materials used in the present invention all have good thermal stability, are non-toxic and non-volatile, are beneficial to environmental protection and the health of operators, have high production efficiency, and meet the requirements of green production.
具体实施方式 Detailed ways
下面结合具体实施例,进一步阐述本发明,应理解,这些实例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作工作改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art may make changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.
实施例1:Example 1:
一种淀粉基絮凝剂的制备方法,包括下列步骤:A preparation method of starch-based flocculant, comprising the following steps:
1)将淀粉(玉米淀粉)置于60Co-γ辐照场中,在有氧条件下(如在空气条件下)进行辐照,辐照剂量为6KGy(辐射剂量固定,则时间都是固定的),使得淀粉产生自由基,得到预辐照淀粉;所述淀粉为玉米淀粉,粘度46mp·s,含水率13.14wt%;1) Put starch (corn starch) in the 60 Co-γ irradiation field, and irradiate under aerobic conditions (such as under air conditions), and the irradiation dose is 6KGy (the radiation dose is fixed, and the time is fixed) ), so that the starch produces free radicals to obtain pre-irradiated starch; the starch is cornstarch, with a viscosity of 46mp·s and a water content of 13.14wt%;
2)按接枝单体的加入量为预辐照淀粉质量的100%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水(去离子水)的质量比为1∶1,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵,丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为5∶5;2) be 100% of pre-irradiated starch quality by the add-on of grafted monomer, select pre-irradiated starch and grafted monomer; Be 1: 1 by the mass ratio of pre-irradiated starch and water (deionized water) , choose water; Wherein, grafting monomer is acrylamide and acryloyloxyethyltrimethylammonium chloride, and the mass ratio of acrylamide and acryloyloxyethyltrimethylammonium chloride is 5:5;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波2.0min(每次微波时间为20s,间歇5s;总共微波6次,总共微波时间为2.0min),使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the evenly stirred mixture in a microwave oven for 2.0 min intermittent microwaves (each microwave time is 20 s, intermittent 5 s; a total of 6 microwave times, a total microwave time of 2.0 min), so that the starch free radicals and the grafted monomers Active groups react to generate grafted starch;
4)将微波后的接枝淀粉在100℃条件下烘焙7小时,经粉碎,得到淀粉基絮凝剂。4) Baking the grafted starch after microwave at 100° C. for 7 hours and crushing to obtain a starch-based flocculant.
所得淀粉基絮凝剂用于处理浓度为200mg/l的活性红染料,在5min内其色度去除率可达87.5%,随着作用时间的延长,其色度最高去除率可达95.8%。说明本实施例得到的淀粉基絮凝剂具有良好的絮凝效果。The obtained starch-based flocculant is used to treat reactive red dye with a concentration of 200 mg/l, and its chromaticity removal rate can reach 87.5% within 5 minutes, and the highest chromaticity removal rate can reach 95.8% with the extension of the action time. It shows that the starch-based flocculant obtained in this example has a good flocculation effect.
实施例2:Example 2:
一种淀粉基絮凝剂的制备方法,包括下列步骤:A preparation method of starch-based flocculant, comprising the following steps:
1)将淀粉置于60Co-γ辐照场中,在有氧条件下(如在空气条件下)进行辐照,辐照剂量为8KGy,使得淀粉产生自由基,得到预辐照淀粉;所述淀粉为玉米淀粉,粘度46mp·s,含水率13.14wt%;1) The starch is placed in a 60 Co-γ irradiation field, and irradiated under aerobic conditions (such as under air conditions), and the irradiation dose is 8KGy, so that the starch generates free radicals to obtain pre-irradiated starch; Said starch is cornstarch, viscosity 46mp s, water content 13.14wt%;
2)按接枝单体的加入量为预辐照淀粉质量的100%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水(去离子水)的质量比为1∶1.5,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵,丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为5∶5;2) be 100% of pre-irradiated starch quality by the add-on of grafted monomer, select pre-irradiated starch and grafted monomer; Be 1: 1.5 by the mass ratio of pre-irradiated starch and water (deionized water) , choose water; Wherein, grafting monomer is acrylamide and acryloyloxyethyltrimethylammonium chloride, and the mass ratio of acrylamide and acryloyloxyethyltrimethylammonium chloride is 5:5;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波140s[每次微波时间为20s,间歇10s;总共微波7次,总共微波时间为140s(即间歇微波140s)],使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the well-stirred mixture in a microwave oven for 140s intermittent microwave [each microwave time is 20s, intermittent 10s; a total of 7 microwaves, a total microwave time of 140s (i.e. intermittent microwave 140s)], so that starch free radicals and grafting The active group on the monomer reacts to generate grafted starch;
4)将微波后的接枝淀粉在80℃条件下烘焙10小时,经粉碎,得到淀粉基絮凝剂。4) Baking the grafted starch after microwave at 80° C. for 10 hours, and crushing to obtain a starch-based flocculant.
所得淀粉基絮凝剂用于处理浓度为200mg/l的活性红染料,在5min内其色度去除率可达89.7%,随着作用时间的延长,其色度最高去除率可达97.4%。说明本实施例得到的淀粉基絮凝剂具有良好的絮凝效果。The obtained starch-based flocculant is used to treat reactive red dye with a concentration of 200 mg/l, and its chromaticity removal rate can reach 89.7% within 5 minutes, and the highest chromaticity removal rate can reach 97.4% with the extension of the action time. It shows that the starch-based flocculant obtained in this example has a good flocculation effect.
实施例3:Example 3:
一种淀粉基絮凝剂的制备方法,包括下列步骤:A preparation method of starch-based flocculant, comprising the following steps:
1)将淀粉置于60Co-γ辐照场中,在有氧条件下进行辐照,辐照剂量为6KGy,使得淀粉产生自由基,得到预辐照淀粉;所述淀粉为玉米淀粉,粘度46mp·s,含水率13.14wt%;1) Starch is placed in the 60 Co-γ irradiation field, irradiated under aerobic conditions, and the irradiation dose is 6KGy, so that the starch generates free radicals to obtain pre-irradiated starch; the starch is corn starch, the viscosity 46mp·s, moisture content 13.14wt%;
2)按接枝单体的加入量为预辐照淀粉质量的70%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水(去离子水)的质量比为1∶2,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵,丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为5∶5;2) be 70% of pre-irradiated starch quality by the add-on of grafted monomer, select pre-irradiated starch and grafted monomer; Be 1: 2 by the mass ratio of pre-irradiated starch and water (deionized water) , choose water; Wherein, grafting monomer is acrylamide and acryloyloxyethyltrimethylammonium chloride, and the mass ratio of acrylamide and acryloyloxyethyltrimethylammonium chloride is 5:5;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波140s[每次微波时间为20s,间歇8s;总共微波7次,总共微波时间为140s(即间歇微波140s)],使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the well-stirred mixture in a microwave oven for 140s intermittent microwave [each microwave time is 20s, intermittent 8s; a total of 7 microwaves, a total microwave time of 140s (i.e. intermittent microwave 140s)], so that starch free radicals and grafting The active group on the monomer reacts to generate grafted starch;
4)将微波后的接枝淀粉在140℃条件下烘焙5小时,经粉碎,得到淀粉基絮凝剂。4) Baking the microwaved grafted starch at 140° C. for 5 hours and crushing to obtain a starch-based flocculant.
所得淀粉基絮凝剂用于处理浓度为200mg/l的活性红染料,在5min内其色度去除率可达86.4%,随着作用时间的延长,其色度最高去除率可达95.2%。说明本实施例得到的淀粉基絮凝剂具有良好的絮凝效果。The obtained starch-based flocculant is used to treat reactive red dye with a concentration of 200 mg/l, and its chromaticity removal rate can reach 86.4% within 5 minutes, and the highest chromaticity removal rate can reach 95.2% with the prolongation of action time. It shows that the starch-based flocculant obtained in this example has a good flocculation effect.
实施例4:Example 4:
一种淀粉基絮凝剂的制备方法,包括下列步骤:A preparation method of starch-based flocculant, comprising the following steps:
1)将淀粉置于60Co-γ辐照场中,在有氧条件下进行辐照,辐照剂量为10KGy,使得淀粉产生自由基,得到预辐照淀粉;所述淀粉为玉米淀粉,粘度46mp·s,含水率13.14wt%;1) Starch is placed in the 60 Co-γ irradiation field, irradiated under aerobic conditions, and the irradiation dose is 10KGy, so that the starch generates free radicals to obtain pre-irradiated starch; the starch is corn starch, the viscosity 46mp·s, moisture content 13.14wt%;
2)按接枝单体的加入量为预辐照淀粉质量的100%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水(去离子水)的质量比为1∶2.5,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵,丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为4∶6;2) be 100% of pre-irradiated starch quality by the add-on of grafted monomer, select pre-irradiated starch and grafted monomer; Be 1: 2.5 by the mass ratio of pre-irradiated starch and water (deionized water) , choose water; Wherein, grafting monomer is acrylamide and acryloyloxyethyltrimethylammonium chloride, and the mass ratio of acrylamide and acryloyloxyethyltrimethylammonium chloride is 4: 6;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波140s(每次微波时间为20s,间歇5s;总共微波7次),使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the well-stirred mixture in a microwave oven for 140s of microwave intermittently (each microwave time is 20s, intermittent 5s; a total of 7 microwaves), so that the starch free radicals react with the active groups on the grafted monomers to generate grafts starch;
4)将微波后的接枝淀粉在140℃条件下烘焙10小时,经粉碎,得到淀粉基絮凝剂。4) Baking the grafted starch after microwave at 140° C. for 10 hours, and crushing to obtain a starch-based flocculant.
所得淀粉基絮凝剂用于处理浓度为200mg/l的活性红染料,在5min内其色度去除率可达87.7%,随着作用时间的延长,其色度最高去除率可达97.9%。说明本实施例得到的淀粉基絮凝剂具有良好的絮凝效果。The obtained starch-based flocculant is used to treat reactive red dye with a concentration of 200 mg/l, and its chromaticity removal rate can reach 87.7% within 5 minutes, and the highest chromaticity removal rate can reach 97.9% as the action time prolongs. It shows that the starch-based flocculant obtained in this example has a good flocculation effect.
实施例5:Example 5:
一种淀粉基絮凝剂的制备方法,包括下列步骤:A preparation method of starch-based flocculant, comprising the following steps:
1)将淀粉(小麦淀粉)置于60Co-γ辐照场中,在有氧条件下进行辐照,辐照剂量为4KGy,使得淀粉产生自由基,得到预辐照淀粉;1) Place starch (wheat starch) in a 60 Co-γ irradiation field and irradiate under aerobic conditions with an irradiation dose of 4KGy to make the starch generate free radicals and obtain pre-irradiated starch;
2)按接枝单体的加入量为预辐照淀粉质量的50%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水的质量比为1∶1,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵(丙烯酰氧乙基三甲基氯化铵为DAC),丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为3∶7;2) be 50% of pre-irradiated starch quality by the add-on of grafted monomer, select pre-irradiated starch and grafted monomer; Be 1: 1 by the mass ratio of pre-irradiated starch and water, choose water; Wherein , the grafting monomers are acrylamide and acryloyloxyethyltrimethylammonium chloride (acryloyloxyethyltrimethylammonium chloride is DAC), acrylamide and acryloyloxyethyltrimethylammonium chloride The mass ratio is 3:7;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波1min(每次微波时间为10s,间歇5s,总共微波6次),使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the evenly stirred mixture in a microwave oven for 1 minute and microwave intermittently (each microwave time is 10 s, intermittent 5 s, microwave 6 times in total), so that the starch free radicals react with the active groups on the grafted monomers to generate grafts. starch;
4)将微波后的接枝淀粉在80℃条件下烘焙5小时,经粉碎,得到淀粉基絮凝剂。4) Baking the grafted starch after microwave at 80° C. for 5 hours, and crushing to obtain a starch-based flocculant.
所得淀粉基絮凝剂用于处理浓度为200mg/l的活性红染料,在5min内其色度去除率可达86.0%,随着作用时间的延长,其色度最高去除率可达96.0%。说明本实施例得到的淀粉基絮凝剂具有良好的絮凝效果。The obtained starch-based flocculant is used to treat reactive red dye with a concentration of 200 mg/l, and its chroma removal rate can reach 86.0% within 5 minutes, and the highest chroma removal rate can reach 96.0% with the prolongation of action time. It shows that the starch-based flocculant obtained in this example has a good flocculation effect.
实施例6:Embodiment 6:
一种淀粉基絮凝剂的制备方法,包括下列步骤:A preparation method of starch-based flocculant, comprising the following steps:
1)将淀粉(马铃薯淀粉)置于60Co-γ辐照场中,在有氧条件下进行辐照,辐照剂量为10KGy,使得淀粉产生自由基,得到预辐照淀粉;1) Place starch (potato starch) in a 60 Co-γ irradiation field and irradiate under aerobic conditions with an irradiation dose of 10KGy to make the starch generate free radicals and obtain pre-irradiated starch;
2)按接枝单体的加入量为预辐照淀粉质量的60%,选取预辐照淀粉和接枝单体;按预辐照淀粉与水的质量比为1∶3,选取水;其中,接枝单体为丙烯酰胺和丙烯酰氧乙基三甲基氯化铵(丙烯酰氧乙基三甲基氯化铵为DAC),丙烯酰胺与丙烯酰氧乙基三甲基氯化铵的质量比为7∶3;2) be 60% of pre-irradiated starch quality by the add-on of grafted monomer, select pre-irradiated starch and grafted monomer; Be 1: 3 by the mass ratio of pre-irradiated starch and water, choose water; Wherein , the grafting monomers are acrylamide and acryloyloxyethyltrimethylammonium chloride (acryloyloxyethyltrimethylammonium chloride is DAC), acrylamide and acryloyloxyethyltrimethylammonium chloride The mass ratio is 7:3;
将预辐照淀粉置于混合器内,将接枝单体置于混合器内,并加入水(去离子水),开动机器搅拌,直至搅拌均匀,得到混合物;Put the pre-irradiated starch in the mixer, put the grafted monomer in the mixer, add water (deionized water), start the machine to stir until it is evenly stirred, and obtain the mixture;
3)将搅拌均匀的混合物置于微波炉中间歇微波3min(每次微波时间为22.5s,间歇15s,总共微波8次),使淀粉自由基与接枝单体上的活性基团反应,生成接枝淀粉;3) Place the well-stirred mixture in a microwave oven for 3 minutes of microwave intermittently (each microwave time is 22.5 s, intermittent 15 s, microwave 8 times in total), so that the starch free radicals react with the active groups on the grafted monomers to generate grafts. Amylopectin;
4)将微波后的接枝淀粉在90℃条件下烘焙6小时,经粉碎,得到淀粉基絮凝剂。4) Baking the grafted starch after microwave at 90° C. for 6 hours and crushing to obtain a starch-based flocculant.
所得淀粉基絮凝剂用于处理浓度为200mg/l的活性红染料,在5min内其色度去除率可达87.0%,随着作用时间的延长,其色度最高去除率可达97.0%。说明本实施例得到的淀粉基絮凝剂具有良好的絮凝效果。The obtained starch-based flocculant is used to treat reactive red dye with a concentration of 200 mg/l, and its chromaticity removal rate can reach 87.0% within 5 minutes, and the highest chromaticity removal rate can reach 97.0% with the prolongation of the action time. It shows that the starch-based flocculant obtained in this example has a good flocculation effect.
其他种类淀粉亦能通过本发明实现,在此不一一操作。本发明所列举的各原料以及各原料的上下限取值,以及各工艺参数的上下限取值,都能实现本发明,在此不一一列举实施例。Other kinds of starches can also be realized by the present invention, and they are not handled one by one here. Each raw material listed in the present invention, the upper and lower limits of each raw material, and the upper and lower limits of each process parameter can realize the present invention, and the embodiments are not listed one by one here.
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