CN103755969A - Chitosan and poly-dimethyl diallyl ammonium chloride compound and preparation method thereof - Google Patents
Chitosan and poly-dimethyl diallyl ammonium chloride compound and preparation method thereof Download PDFInfo
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- CN103755969A CN103755969A CN201410014611.1A CN201410014611A CN103755969A CN 103755969 A CN103755969 A CN 103755969A CN 201410014611 A CN201410014611 A CN 201410014611A CN 103755969 A CN103755969 A CN 103755969A
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- Prior art keywords
- ammonium chloride
- chitosan
- dimethyl diallyl
- diallyl ammonium
- poly dimethyl
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- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 title claims abstract description 58
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 229960000583 acetic acid Drugs 0.000 claims abstract description 14
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 239000003999 initiator Substances 0.000 claims abstract description 11
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 20
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 12
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000178 monomer Substances 0.000 claims description 12
- 239000003352 sequestering agent Substances 0.000 claims description 12
- 239000004160 Ammonium persulphate Substances 0.000 claims description 7
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000010189 synthetic method Methods 0.000 claims description 2
- 239000010865 sewage Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- 229920002101 Chitin Polymers 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 3
- 230000000274 adsorptive effect Effects 0.000 abstract 1
- 230000003311 flocculating effect Effects 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a chitosan and poly-dimethyl diallyl ammonium chloride compound, comprising the following raw materials in parts by weight: 1 part of chitosan, and 3-8 parts of poly-dimethyl diallyl ammonium chloride. The invention also discloses a preparation method of the chitosan and poly-dimethyl diallyl ammonium chloride compound. The method comprises the following steps: adding glacial acetic acid to a reaction kettle; adding the chitosan, and stirring to be completely dissolved; charging nitrogen to the reaction kettle, adding the dimethyl diallyl ammonium chloride; adding an initiator and preserving the heat to 30-70 DEG C, so as to obtain the compound, wherein the reaction time is 3-6h. By adopting the method, the compound is prepared by synthesizing the chitosan and the poly-dimethyl diallyl ammonium chloride, and the chitosan and poly-dimethyl diallyl ammonium chloride compound has strong adsorptive property and flocculating performance, and can be used as an ideal chemical medicine in a sewage treatment industry; as a derivative of chitin, so that the chitosan is wide in source, abundant in storage amount, low in cost, and free of secondary pollution. Thus, the compound is applicable to great popularization in the sewage treatment industry.
Description
Technical field
The present invention relates to a kind of sewage disposal chemical complex and preparation method, relate in particular to a kind of chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture and preparation method.
Background technology
Poly Dimethyl Diallyl Ammonium Chloride is strong cation polyelectrolyte, outward appearance is colourless to light yellow viscous liquid, have safe, nontoxic, soluble in water, nonflammable, cohesive force is strong, stability to hydrolysis good, do not become gel, pH value is changed to insensitive, to have chlorine resistance feature, more as cationic coagulant application at sewage treatment industry.
But a lot of complicated components of waste water control pharmaceutical chemicals take Poly Dimethyl Diallyl Ammonium Chloride as cationic coagulant at present, but also need the raw material of other higher cost, so cause the production cost of finished product medicine higher, in sewage disposal demand, more and more widely in situation, traditional chemical medicine is not easy to popularize.
Summary of the invention
Object of the present invention be just to provide in order to address the above problem a kind of excellent property, cost lower, be easy to the chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture and the preparation method that promote.
The present invention is achieved through the following technical solutions above-mentioned purpose:
A kind of chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture, comprise chitosan and Poly Dimethyl Diallyl Ammonium Chloride, and the mass parts of described chitosan is 1 part, and the mass parts of described Poly Dimethyl Diallyl Ammonium Chloride is 3～8 parts.
Chitosan is the derivative generating after chitin part deacetylate; chemical name is: β-(1; 4)-2-amino-2-deoxy-D-Glucose; research is found, on chitosan molecule chain, distributing many hydroxyls, amino also have part N-ethanoyl; the existence of these groups makes chitosan show the chemical property of many uniquenesses; introduce after strong electropositive quaternary ammonium salt group, positively charged ion intensity improves greatly, can strengthen Adsorption and flocculation performance.After chitosan and Poly Dimethyl Diallyl Ammonium Chloride is synthetic, chitosan has been introduced cation group, and Adsorption and flocculation performance strengthens greatly.
Particularly, the mass parts of described Poly Dimethyl Diallyl Ammonium Chloride is 5 parts.
A preparation method for chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture, comprises the following steps:
(1) in reactor, add Glacial acetic acid, then add the chitosan of 1 mass parts, be stirred to completely and dissolve;
(2) in reactor, be filled with nitrogen, under nitrogen protection, add the Poly Dimethyl Diallyl Ammonium Chloride of 3～8 mass parts;
(3) add initiator, maintain the temperature at 30 ℃～70 ℃, the reaction times is 3～6h, obtains chitosan and reacts the mixture generating with Poly Dimethyl Diallyl Ammonium Chloride.
Particularly, the concentration of described Glacial acetic acid is 5%.
In described step (3), described initiator is ammonium persulphate; In described step (3), maintain the temperature at 40 ℃～60 ℃, the reaction times is 4～5h.
More specifically, in described step (2), the synthetic method of described Poly Dimethyl Diallyl Ammonium Chloride is as follows: in polymeric kettle, add dimethyldiallylammonchloride chloride monomer, by diluted acid adjusting reaction system, pH is extremely neutral, after stirring, start heating, when temperature rises to 60～70 ℃, add 1/8 in 0.008% the sequestrant sodium ethylene diamine tetracetate that accounts for dimethyldiallylammonchloride chloride monomer total mass, maintain the temperature at 60～70 ℃ of regions, then in 3h, drip continuously remaining sequestrant sodium ethylene diamine tetracetate, insulation reaction 2h, after reaction finishes, cool and obtain Poly Dimethyl Diallyl Ammonium Chloride.
Beneficial effect of the present invention is:
The present invention prepares mixture by synthetic to chitosan and Poly Dimethyl Diallyl Ammonium Chloride, and its Adsorption and flocculation performance is extremely strong, can be used as the desirable pharmaceutical chemicals of sewage treatment industry; Chitosan is as the derivative of chitin, its wide material sources, and reserves are abundant, with low cost, are difficult for causing secondary pollution, so that this mixture is suitable in sewage treatment industry large-scale popularization is universal.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
Prepare according to the following steps chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture:
(1) prepare Poly Dimethyl Diallyl Ammonium Chloride: in polymeric kettle, add dimethyldiallylammonchloride chloride monomer, by diluted acid adjusting reaction system, pH is extremely neutral, after stirring, start heating, when temperature rises to 60～70 ℃, add 1/8 in 0.008% the sequestrant sodium ethylene diamine tetracetate that accounts for dimethyldiallylammonchloride chloride monomer total mass, maintain the temperature at 60～70 ℃ of regions, then in 3h, drip continuously remaining sequestrant sodium ethylene diamine tetracetate, insulation reaction 2h, after reaction finishes, cool and obtain Poly Dimethyl Diallyl Ammonium Chloride,
(2) in reactor, adding concentration is 5% Glacial acetic acid, then adds the chitosan of 1 mass parts, is stirred to completely and dissolves, and the add-on of Glacial acetic acid can completely be dissolved and be limited with chitosan, specifically determines as required;
(3) in reactor, be filled with nitrogen, under nitrogen protection, add the Poly Dimethyl Diallyl Ammonium Chloride of 3 mass parts;
(4) add initiator ammonium persulfate, maintain the temperature at 30 ℃～40 ℃, reaction times is 3～4h, obtain chitosan and react the mixture generating with Poly Dimethyl Diallyl Ammonium Chloride, the add-on of ammonium persulphate is reacted and is limited with Poly Dimethyl Diallyl Ammonium Chloride can cause chitosan, specifically determines as required.
Embodiment 2:
Prepare according to the following steps chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture:
(1) prepare Poly Dimethyl Diallyl Ammonium Chloride: in polymeric kettle, add dimethyldiallylammonchloride chloride monomer, by diluted acid adjusting reaction system, pH is extremely neutral, after stirring, start heating, when temperature rises to 60～70 ℃, add 1/8 in 0.008% the sequestrant sodium ethylene diamine tetracetate that accounts for dimethyldiallylammonchloride chloride monomer total mass, maintain the temperature at 60～70 ℃ of regions, then in 3h, drip continuously remaining sequestrant sodium ethylene diamine tetracetate, insulation reaction 2h, after reaction finishes, cool and obtain Poly Dimethyl Diallyl Ammonium Chloride,
(2) in reactor, adding concentration is 5% Glacial acetic acid, then adds the chitosan of 1 mass parts, is stirred to completely and dissolves, and the add-on of Glacial acetic acid can completely be dissolved and be limited with chitosan, specifically determines as required;
(3) in reactor, be filled with nitrogen, under nitrogen protection, add the Poly Dimethyl Diallyl Ammonium Chloride of 5 mass parts;
(4) add initiator ammonium persulfate, maintain the temperature at 40 ℃～50 ℃, reaction times is 4～5h, obtain chitosan and react the mixture generating with Poly Dimethyl Diallyl Ammonium Chloride, the add-on of ammonium persulphate is reacted and is limited with Poly Dimethyl Diallyl Ammonium Chloride can cause chitosan, specifically determines as required.
Embodiment 3:
Prepare according to the following steps chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture:
(1) prepare Poly Dimethyl Diallyl Ammonium Chloride: in polymeric kettle, add dimethyldiallylammonchloride chloride monomer, by diluted acid adjusting reaction system, pH is extremely neutral, after stirring, start heating, when temperature rises to 60～70 ℃, add 1/8 in 0.008% the sequestrant sodium ethylene diamine tetracetate that accounts for dimethyldiallylammonchloride chloride monomer total mass, maintain the temperature at 60～70 ℃ of regions, then in 3h, drip continuously remaining sequestrant sodium ethylene diamine tetracetate, insulation reaction 2h, after reaction finishes, cool and obtain Poly Dimethyl Diallyl Ammonium Chloride,
(2) in reactor, adding concentration is 5% Glacial acetic acid, then adds the chitosan of 1 mass parts, is stirred to completely and dissolves, and the add-on of Glacial acetic acid can completely be dissolved and be limited with chitosan, specifically determines as required;
(3) in reactor, be filled with nitrogen, under nitrogen protection, add the Poly Dimethyl Diallyl Ammonium Chloride of 6 mass parts;
(4) add initiator ammonium persulfate, maintain the temperature at 50 ℃～60 ℃, reaction times is 5～6h, obtain chitosan and react the mixture generating with Poly Dimethyl Diallyl Ammonium Chloride, the add-on of ammonium persulphate is reacted and is limited with Poly Dimethyl Diallyl Ammonium Chloride can cause chitosan, specifically determines as required.
Embodiment 4:
Prepare according to the following steps chitosan and Poly Dimethyl Diallyl Ammonium Chloride mixture:
(1) prepare Poly Dimethyl Diallyl Ammonium Chloride: in polymeric kettle, add dimethyldiallylammonchloride chloride monomer, by diluted acid adjusting reaction system, pH is extremely neutral, after stirring, start heating, when temperature rises to 60～70 ℃, add 1/8 in 0.008% the sequestrant sodium ethylene diamine tetracetate that accounts for dimethyldiallylammonchloride chloride monomer total mass, maintain the temperature at 60～70 ℃ of regions, then in 3h, drip continuously remaining sequestrant sodium ethylene diamine tetracetate, insulation reaction 2h, after reaction finishes, cool and obtain Poly Dimethyl Diallyl Ammonium Chloride,
(2) in reactor, adding concentration is 5% Glacial acetic acid, then adds the chitosan of 1 mass parts, is stirred to completely and dissolves, and the add-on of Glacial acetic acid can completely be dissolved and be limited with chitosan, specifically determines as required;
(3) in reactor, be filled with nitrogen, under nitrogen protection, add the Poly Dimethyl Diallyl Ammonium Chloride of 8 mass parts;
(4) add initiator ammonium persulfate, maintain the temperature at 60 ℃～70 ℃, reaction times is 5h, obtain chitosan and react the mixture generating with Poly Dimethyl Diallyl Ammonium Chloride, the add-on of ammonium persulphate is reacted and is limited with Poly Dimethyl Diallyl Ammonium Chloride can cause chitosan, specifically determines as required.
Above-described embodiment is preferred embodiment of the present invention, is not the restriction to technical solution of the present invention, such as: Glacial acetic acid concentration can also be greater than or less than 5%; Initiator also can be with other initiator beyond ammonium persulphate; Poly Dimethyl Diallyl Ammonium Chloride also can adopt other method preparation; As long as the technical scheme that can realize on the basis of above-described embodiment without creative work, all should be considered as falling within the scope of the rights protection of patent of the present invention.
Claims (7)
1. chitosan and a Poly Dimethyl Diallyl Ammonium Chloride mixture, is characterized in that: comprise chitosan and Poly Dimethyl Diallyl Ammonium Chloride, the mass parts of described chitosan is 1 part, and the mass parts of described Poly Dimethyl Diallyl Ammonium Chloride is 3～8 parts.
2. chitosan according to claim 1 and Poly Dimethyl Diallyl Ammonium Chloride mixture, is characterized in that: the mass parts of described Poly Dimethyl Diallyl Ammonium Chloride is 5 parts.
3. a preparation method for chitosan as claimed in claim 1 and Poly Dimethyl Diallyl Ammonium Chloride mixture, is characterized in that: comprise the following steps:
(1) in reactor, add Glacial acetic acid, then add the chitosan of 1 mass parts, be stirred to completely and dissolve;
(2) in reactor, be filled with nitrogen, under nitrogen protection, add the Poly Dimethyl Diallyl Ammonium Chloride of 3～8 mass parts;
(3) add initiator, maintain the temperature at 30 ℃～70 ℃, the reaction times is 3～6h, obtains chitosan and reacts the mixture generating with Poly Dimethyl Diallyl Ammonium Chloride.
4. thing preparation method according to claim 3, is characterized in that: in described step (1), the concentration of described Glacial acetic acid is 5%.
5. thing preparation method according to claim 3, is characterized in that: in described step (3), described initiator is ammonium persulphate.
6. according to the thing preparation method described in claim 3 or 5, it is characterized in that: in described step (3), maintain the temperature at 40 ℃～60 ℃, the reaction times is 4～5h.
7. thing preparation method according to claim 3, it is characterized in that: in described step (2), the synthetic method of described Poly Dimethyl Diallyl Ammonium Chloride is as follows: in polymeric kettle, add dimethyldiallylammonchloride chloride monomer, by diluted acid adjusting reaction system, pH is extremely neutral, after stirring, start heating, when temperature rises to 60～70 ℃, add 1/8 in 0.008% the sequestrant sodium ethylene diamine tetracetate that accounts for dimethyldiallylammonchloride chloride monomer total mass, maintain the temperature at 60～70 ℃ of regions, then in 3h, drip continuously remaining sequestrant sodium ethylene diamine tetracetate, insulation reaction 2h, after reaction finishes, cool and obtain Poly Dimethyl Diallyl Ammonium Chloride.
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| CN201410014611.1A CN103755969A (en) | 2014-01-14 | 2014-01-14 | Chitosan and poly-dimethyl diallyl ammonium chloride compound and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858848A (en) * | 2016-03-28 | 2016-08-17 | 黄忠卫 | Clarificant and preparation method thereof |
| CN107417943A (en) * | 2017-08-30 | 2017-12-01 | 武汉理工大学 | A kind of chitosan-based anion-exchange membrane of high intensity and preparation method thereof |
| CN108017128A (en) * | 2017-11-29 | 2018-05-11 | 无锡锐众环保科技有限公司 | A kind of macromolecular multi-component flocculation modifying agent, its preparation method and application |
| CN108192309A (en) * | 2018-04-04 | 2018-06-22 | 刘凡领 | A kind of preparation method of artificial marble |
| CN109721142A (en) * | 2019-02-20 | 2019-05-07 | 沈阳振兴环保有限公司 | A kind of water purification agent composition and its preparation method and application |
| CN113955837A (en) * | 2021-10-18 | 2022-01-21 | 神美科技有限公司 | Inorganic-organic composite polymer defluorination flocculant for water treatment and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105858848A (en) * | 2016-03-28 | 2016-08-17 | 黄忠卫 | Clarificant and preparation method thereof |
| CN107417943A (en) * | 2017-08-30 | 2017-12-01 | 武汉理工大学 | A kind of chitosan-based anion-exchange membrane of high intensity and preparation method thereof |
| CN108017128A (en) * | 2017-11-29 | 2018-05-11 | 无锡锐众环保科技有限公司 | A kind of macromolecular multi-component flocculation modifying agent, its preparation method and application |
| CN108192309A (en) * | 2018-04-04 | 2018-06-22 | 刘凡领 | A kind of preparation method of artificial marble |
| CN109721142A (en) * | 2019-02-20 | 2019-05-07 | 沈阳振兴环保有限公司 | A kind of water purification agent composition and its preparation method and application |
| CN113955837A (en) * | 2021-10-18 | 2022-01-21 | 神美科技有限公司 | Inorganic-organic composite polymer defluorination flocculant for water treatment and preparation method thereof |
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Application publication date: 20140430 |