CN107162149B - A kind of preparation method of anionic acrylamide flocculating agent - Google Patents
A kind of preparation method of anionic acrylamide flocculating agent Download PDFInfo
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- CN107162149B CN107162149B CN201710558497.2A CN201710558497A CN107162149B CN 107162149 B CN107162149 B CN 107162149B CN 201710558497 A CN201710558497 A CN 201710558497A CN 107162149 B CN107162149 B CN 107162149B
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- Prior art keywords
- starch
- preparation
- flocculating agent
- water
- certain amount
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- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 125000000129 anionic group Chemical group 0.000 title claims abstract description 23
- 239000008394 flocculating agent Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920002472 Starch Polymers 0.000 claims abstract description 49
- 235000019698 starch Nutrition 0.000 claims abstract description 49
- 239000008107 starch Substances 0.000 claims abstract description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 11
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 11
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 11
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940106681 chloroacetic acid Drugs 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 229920002261 Corn starch Polymers 0.000 claims description 3
- 239000008120 corn starch Substances 0.000 claims description 3
- 229940099112 cornstarch Drugs 0.000 claims description 3
- 238000010894 electron beam technology Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920001592 potato starch Polymers 0.000 claims description 2
- 244000151018 Maranta arundinacea Species 0.000 claims 1
- 235000010804 Maranta arundinacea Nutrition 0.000 claims 1
- 235000012419 Thalia geniculata Nutrition 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 description 7
- 229920000881 Modified starch Polymers 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 235000019426 modified starch Nutrition 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000004368 Modified starch Substances 0.000 description 2
- -1 anionic propylene Amide Chemical class 0.000 description 2
- 229920006320 anionic starch Polymers 0.000 description 2
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 2
- 230000003311 flocculating effect Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to prepare anionic flocculant technical field.A kind of preparation method of anionic acrylamide flocculating agent, it is characterised in that include the following steps: 1) to take a certain amount of irradiated starch, be dissolved in water, after agitating and heating gelatinization, obtain gelatinized starch, for use；2) a certain amount of sodium hydrate solid is weighed, after being dissolved in water, obtains sodium hydroxide solution；It pours into gelatinized starch, alkalizes, obtain alkalization starch；3) by after system temperature is down to 60 DEG C in 2) step, a certain amount of chloroacetic acid solid is weighed, after being dissolved in water, pours into alkalization starch, continues constant temperature stirring after a certain period of time；4) a certain amount of acrylamide solid is taken, after water dissolution is added, is added in the gelatinized starch that step 3) obtains, constant temperature stirring is kept；5) a certain amount of dissolved ammonium ceric nitrate catalysis reaction is added, obtains anionic acrylamide flocculating agent.This method has that simple process, investment goods are few, advantage of lower cost, and can obtain good using effect.
Description
Technical field
The invention belongs to prepare anionic flocculant technical field, wad a quilt with cotton more particularly to a kind of anionic acrylamide
The preparation method of solidifying agent.
Background technique
Acrylamide is a kind of unsaturated amine, and it is the monomer of organic material synthesis that monomer, which is colorless and transparent flaky crystal,
It is commonly used to do the monomer material of graft copolymerization.Starch and its derivative are cheap because source is wide, environmentally safe etc. excellent
Point becomes the important substance of sewage treatment, and modified starch has more superior performance, common cationic compared with native starch
Starch derivative flocculant, it is nontoxic, degradable, charging neutrality and adsorption bridging can be played with particle in water, be usually used in locating
Reason carries the sewage of negative electrical charge.Anionic starch flocculant can be used for sewage treatment, it and heavy metal ion generate hardly possible
Molten object precipitating, Cong Shuizhong heavy-metal ion removal.Anionic starch ether once caused in multiple countries such as Japan, the U.S., Germany
Comparable attention is crossed, a variety of modified starch flocculants have been obtained.
The present invention increases the flocculating function of starch by grafting chloroacetic acid and acrylamide, for handling some dyes
Expect that sewage has good result.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of anionic acrylamide flocculating agent, this method has work
Skill is simple, investment goods are few, advantage of lower cost, and can obtain good using effect.
To achieve the above object, the technical scheme adopted by the invention is that: a kind of anionic acrylamide flocculating agent
Preparation method, it is characterised in that include the following steps:
1) a certain amount of irradiated starch is taken, is dissolved in water, after agitating and heating gelatinization, obtains gelatinized starch, for use；
2) a certain amount of sodium hydrate solid is weighed, after being dissolved in water, obtains sodium hydroxide solution；Pour into gelatinized starch
It is interior, it alkalizes, obtains alkalization starch (continuing constant temperature stirring)；
3) by after system temperature is down to 60 DEG C in 2) step, a certain amount of chloroacetic acid solid is weighed, after being dissolved in water,
Enter to alkalize in starch, continues constant temperature stirring after a certain period of time；
4) a certain amount of acrylamide solid is taken, after water dissolution is added, is added in the gelatinized starch that step 3) obtains, protects
Hold constant temperature stirring；
5) a certain amount of dissolved ammonium ceric nitrate catalysis reaction is added, obtains anionic acrylamide flocculating agent.
The preparation of irradiated starch described in step 1) are as follows: weigh starch, irradiated under room temperature, irradiation bomb, irradiation dose is
40kgy；The irradiation bomb is60Any one in Co- gamma-rays, x-ray, electron beam etc., preferably60Co- gamma-rays.
The starch is one of cornstarch, wheaten starch, tapioca, potato starch etc..
Irradiated starch in step 1), water proportion be 25g:110mL.
In step 1), heating temperature is 95 DEG C, time 30min.
In step 2), it is 0.7g:25g by the proportion of sodium hydroxide solution, irradiated starch, chooses sodium hydroxide solution；Hydrogen
The concentration of sodium hydroxide solution is 10wt%.
In step 2), alkalization time 15min.
In step 3), it is 1.5g:25g by the proportion of chloroacetic acid solid, irradiated starch, chooses chloroacetic acid solid；One
Monoxone solid, water proportion be 1.5g:10mL, continuations constant temperature mixing time be 30min.
In step 4), it is 10.32g:25g by the proportion of acrylamide solid, irradiated starch, chooses acrylamide solid
(acrylamide solid and irradiated starch equimolar ratio)；Acrylamide solid, water proportion be 10.32g:20mL.
In step 5), it is 0.75g:25g by the proportion of ammonium ceric nitrate, irradiated starch, chooses ammonium ceric nitrate；Ammonium ceric nitrate,
The proportion of water is 0.75g:15mL.
Anionic flocculant of the invention is suitable for dye wastewater processing aspect.
Beneficial effects of the present invention: the 1) advantage 2 that starch-based flocculant has raw material sources wide, cheap) with starch
For basic raw material, product is safety low-poison, not will cause secondary pollution 3) there are better effects for processing dye wastewater.
Specific embodiment
Present invention will be further explained below with reference to specific examples, it should be appreciated that these examples be merely to illustrate the present invention and
It is not used in and limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
It can make work change to the present invention or modification, such equivalent forms are equally fallen within defined by the application the appended claims
Range.
Embodiment 1:
A kind of preparation method of anionic acrylamide flocculating agent, includes the following steps:
1) 25g irradiated starch is weighed, the dissolution of 110mL water is added, (water bath with thermostatic control heating, temperature are after agitating and heating gelatinization
95 DEG C, gelatinized starch 30min), gelatinized starch is obtained, for use；
The preparation of the irradiated starch are as follows: weigh cornstarch, irradiated under room temperature, irradiation bomb, irradiation dose is
40kgy；The irradiation bomb is60Co- gamma-rays；
2) after gelatinization is completed, 0.7g, 10wt%NaOH solution are configured, is added in flask, alkalize starch 15min, obtains
Alkalize starch.
3) water bath with thermostatic control heating temperature is reduced to after 60 DEG C, is weighed 1.5g chloroacetic acid solid { ClCH2COOH }, is added 10mL
Water dissolution, is poured into flask, keeps constant temperature stirring (60 DEG C of constant temperature stirrings) 30min；
4) 10.32g acrylamide (acrylamide solid) is weighed, the water dissolution of 20mL is added, is added in flask and { is added
In the gelatinized starch obtained to step 3) }, keep constant temperature stirring (60 DEG C of constant temperature stirrings)；
5) 0.75g ammonium ceric nitrate is weighed, is dissolved with the water of 15ml, ceric ammonium nitrate solution is added dropwise instead using buret
It answers in system, keeps constant temperature stirring (60 DEG C of constant temperature stirrings)；It is dripped off to ammonium ceric nitrate, stops heating, obtain anionic propylene
Amide flocculant.
Gained anionic acrylamide flocculant has preferable flocculating effect.By flocculant process metal ion sewage,
It uses coloration, COD etc. to test to it, show that it is launched than being 5g/L.Untreated sewage coloration is 1300 times, processing
Coloration is 34 times afterwards.Untreated sewage COD is 2750mg/L, and COD is 140mg/L after processing.Illustrate: yin
Acrylamide flocculant has good using effect.
Claims (9)
1. a kind of preparation method of anionic acrylamide flocculating agent, it is characterised in that include the following steps:
1) a certain amount of irradiated starch is taken, is dissolved in water, after agitating and heating gelatinization, obtains gelatinized starch, for use；
2) a certain amount of sodium hydrate solid is weighed, after being dissolved in water, obtains sodium hydroxide solution；It pours into gelatinized starch, into
Row alkalization obtains alkalization starch；
3) by after system temperature is down to 60 DEG C in 2) step, a certain amount of chloroacetic acid solid is weighed, after being dissolved in water, pours into alkali
Change in starch, continues constant temperature stirring after a certain period of time；
4) a certain amount of acrylamide solid is taken, after water dissolution is added, is added in the gelatinized starch that step 3) obtains, keeps permanent
Temperature stirring；
5) a certain amount of dissolved ammonium ceric nitrate catalysis reaction is added, obtains anionic acrylamide flocculating agent.
2. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
1) preparation of the irradiated starch described in are as follows: starch is weighed, is irradiated under room temperature, irradiation bomb, irradiation dose 40kgy；The spoke
It is according to source60Co- gamma-rays, x-ray, any one in electron beam；The starch is cornstarch, wheaten starch, para arrowroot
One of powder, potato starch.
3. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
1) irradiated starch in, water proportion be 25g:110mL.
4. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
1) in, heating temperature is 95 DEG C, time 30min.
5. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
2) in, it is 0.7g:25g by the proportion of sodium hydroxide solution, irradiated starch, chooses sodium hydroxide solution；Sodium hydroxide solution
Concentration is 10wt%.
6. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
2) in, alkalization time 15min.
7. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
3) in, it is 1.5g:25g by the proportion of chloroacetic acid solid, irradiated starch, chooses chloroacetic acid solid；Chloroacetic acid solid, water
Proportion be 1.5g:10mL, continuations constant temperature mixing time be 30min.
8. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
4) in, it is 10.32g:25g by the proportion of acrylamide solid, irradiated starch, chooses acrylamide solid；Acrylamide solid,
The proportion of water is 10.32g:20mL.
9. a kind of preparation method of anionic acrylamide flocculating agent according to claim 1, it is characterised in that: step
5) in, it is 0.75g:25g by the proportion of ammonium ceric nitrate, irradiated starch, chooses ammonium ceric nitrate；Ammonium ceric nitrate, water proportion be
0.75g:15mL.
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| CN107162149B true CN107162149B (en) | 2019-08-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107555568A (en) * | 2017-09-27 | 2018-01-09 | 山东神州翔宇科技集团有限公司 | A kind of pre-gelatinized starch flocculant and preparation method thereof |
| CN108658135A (en) * | 2018-05-06 | 2018-10-16 | 安徽乐金环境科技有限公司 | One kind being based on diatomaceous Water body cleansing agent |
| CN108773860A (en) * | 2018-05-06 | 2018-11-09 | 安徽乐金环境科技有限公司 | A kind of preparation method based on diatomaceous Water body cleansing agent |
| CN108706794A (en) * | 2018-05-06 | 2018-10-26 | 安徽乐金环境科技有限公司 | One kind is based on diatomaceous water body purification filter core and preparation method thereof |
| CN109811353B (en) * | 2019-04-02 | 2021-02-12 | 广州市帝东环保科技有限公司 | Environment-friendly aluminum alloy surface treatment liquid and preparation method thereof |
| CN111908577B (en) * | 2020-07-20 | 2022-04-19 | 重庆工商大学 | Method for synthesizing efficient flocculant through hydrolysis optimization |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121880A (en) * | 2007-08-01 | 2008-02-13 | 成都市互利达实业有限公司 | Natural macromolecule modified starch profile control agent for oil field |
| CN104177635A (en) * | 2014-09-22 | 2014-12-03 | 广西民族大学 | Preparation method of triple cross-linked binary graft copolymer starch |
| CN106699964A (en) * | 2016-11-15 | 2017-05-24 | 湖北兴发化工集团股份有限公司 | Anionic polyacrylamide flocculant, as well as preparation method and application thereof |
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2017
- 2017-07-11 CN CN201710558497.2A patent/CN107162149B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121880A (en) * | 2007-08-01 | 2008-02-13 | 成都市互利达实业有限公司 | Natural macromolecule modified starch profile control agent for oil field |
| CN104177635A (en) * | 2014-09-22 | 2014-12-03 | 广西民族大学 | Preparation method of triple cross-linked binary graft copolymer starch |
| CN106699964A (en) * | 2016-11-15 | 2017-05-24 | 湖北兴发化工集团股份有限公司 | Anionic polyacrylamide flocculant, as well as preparation method and application thereof |
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