CN106349427A - AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method - Google Patents
AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method Download PDFInfo
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- CN106349427A CN106349427A CN201610745063.9A CN201610745063A CN106349427A CN 106349427 A CN106349427 A CN 106349427A CN 201610745063 A CN201610745063 A CN 201610745063A CN 106349427 A CN106349427 A CN 106349427A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- Hydrology & Water Resources (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses an AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method. The method includes steps: S1, adding DAC monomers and AM monomers into a reaction bottle, and stirring to obtain mixed solution; S2, feeding nitrogen into the mixed solution, adding an initiation system, stirring, observing viscosity and temperature changes of the solution, recording a highest temperature value, keeping the temperature at the highest temperature value, and naturally cooling to obtain gel of an AM and DAC copolymer; S3, chopping the gel of the AM and DAC copolymer, and granulating to obtain small-particle-size gel of the AM and DAC copolymer; S4, subjecting the small-particle-size gel of the AM and DAC copolymer to drying, packaging and analyzing to obtain a finished product of the AM and DAC copolymer. The preparation method is simple, feasible, complete in reaction, great in reaction effect and less prone to monomer agglomeration, and the prepared AM and DAC copolymer is high in purity and excellent in flocculation effect.
Description
Technical field
The present invention relates to the preparation method of chemosynthesis technical field, more particularly, to a kind of am and dac copolymer.
Background technology
Since entering 20 century 70s, the development of cationic flocculant assumes obvious growth, U.S., day,
English, Fa Deng state at present in waste water all in a large number using cationic flocculant.Beautiful, Deng state cationic flocculant has accounted for synthesis wadding
The 60% of solidifying agent total amount, and this is still increased for several years with more than 10% speed.But in China, the nearly more than ten years just start to cation
High polymer coagulant is studied although also achieving suitable progress to this research and development, but has been developed into flocculant at present
Species less, therefore, strengthen the development and application research of cationic flocculant, the feedwater production to China and wastewater treatment and
Solid-liquid separation in commercial production has particularly significant meaning.
Content of the invention
The invention aims to shortcoming present in solution prior art, and a kind of am proposing and dac copolymer
Preparation method.
A kind of am and the preparation method of dac copolymer, comprise the following steps:
S1: add acrylyl oxy-ethyl-trimethyl salmiac (dac) monomer in reaction bulb, the reaction outside reaction bulb is filled simultaneously
The temperature put is preset as 5～15 DEG C, after the temperature of question response device reaches, by acrylamide (am) monomer with 1～5g/min's
Speed is added in reaction bulb, opens agitating device, and setting mixing speed is 200～300r/min, it is stirred 10～
20min, obtains mixed solution；
S2: be continually fed into nitrogen 20～40min in above-mentioned mixed solution, then under conditions of being passed through nitrogen, to reaction bulb
Middle addition initiator system, continues to be stirred with the speed of 200～300r/min, and observing response device during 10～30min
The viscosity of middle solution and temperature change, when reaction temperature begins to decline from maximum temperature, record maximum temperature value, and will react
Bottle is transferred in the constant temperature pot that temperature is above-mentioned maximum temperature value, stops being passed through of nitrogen simultaneously, reaction bulb is sealed, and carries out
Insulation operation 1～3 hour, reaction bulb is taken out after terminating by insulation operation, naturally cools to 30～50 DEG C, obtains final product am and dac altogether
The gel of polymers；
S3: the gel of above-mentioned am and dac copolymer is first carried out stripping and slicing, then puts into and carry out pelletize in comminutor, you can obtain
Particle diameter is the gel of the am and dac copolymer of 1～3mm；
S4: above-mentioned particle diameter is the gel drying again of the am and dac copolymer of 1～3mm, packaging, and analysis procedure obtains final product am and dac
Copolymer finished product.
Preferably, described dac monomer and the percentage by weight of am monomer are: dac monomer 10～80%, am monomer 90～
20%, and above-mentioned dac monomer is 100% with the percentage by weight summation of am monomer.
Preferably, described initiator system is Ammonium persulfate .-azodiisobutyronitrile.
Preferably, the consumption of described initiator system is the 0.2～0.5% of dac monomer and am monomer total amount.
Preferably, in described s4 step, the drying temperature of baking operation is 40～60 DEG C.
Preferably, in described s4 step, the drying time of baking operation is 3～6 hours.
A kind of preparation method of am and dac copolymer proposed by the present invention is simple, easy, and the am preparing and dac copolymerization
Carry, on thing strand, the positive charge group that can ionize, water can be ionized into polycation and little anion, can be with
It is scattered in the suspended particles absorption of solution and builds bridge, form extremely strong flocculation, can serve as flocculant, and consumption is less；
The strict addition speed controlling am monomer in preparation process, prevent from rapidly joining the phenomenon that the am monomer leading to reunites it is ensured that
Am reaction completely, is continually fed into nitrogen, makes the oxygen in reaction system cleared it is ensured that reaction system is carried out under anaerobic,
Prevent the generation of side reaction it is ensured that product purity；Holding temperature is determined according to specific experiment situation, it is to avoid differences between batches, enter one
Step improving product purity；The gel of the am and the dac copolymer that are obtained first carried out stripping and slicing put into comminutor again facilitating pelletize
Operation, saves granulation time, improves granulation outcome.
Specific embodiment
With reference to specific embodiment, the present invention is explained further.
Embodiment one
A kind of am proposed by the present invention and the preparation method of dac copolymer, comprise the following steps:
S1: add acrylyl oxy-ethyl-trimethyl salmiac (dac) monomer in reaction bulb, the reaction outside reaction bulb is filled simultaneously
The temperature put is preset as 10 DEG C, after the temperature of question response device reaches, acrylamide (am) monomer is added with the speed of 2g/min
Enter in reaction bulb, open agitating device, setting mixing speed is 250r/min, is stirred 15min, obtains mixed solution；
S2: be continually fed into nitrogen 30min in above-mentioned mixed solution, then under conditions of being passed through nitrogen, add in reaction bulb
Enter ammonium sulfate-azodiisobutyronitrile, continue to be stirred with the speed of 250r/min, and observing response during 10～30min
The viscosity of solution and temperature change in device, when reaction temperature begins to decline from maximum temperature, record maximum temperature value, and will be anti-
In answer bottle to be transferred to constant temperature pot that temperature is above-mentioned maximum temperature value, stop being passed through of nitrogen simultaneously, reaction bulb is sealed, goes forward side by side
Row insulation operation 2 hours, reaction bulb is taken out after terminating by insulation operation, naturally cools to 40 DEG C, obtains final product am and dac copolymer
Gel；
S3: the gel of above-mentioned am and dac copolymer is first carried out stripping and slicing, then puts into and carry out pelletize in comminutor, you can obtain
Particle diameter is the gel of the am and dac copolymer of 2mm；
S4: above-mentioned particle diameter is that the gel of the am and dac copolymer of 2mm is dried 5 hours through 50 DEG C and packaging again, and analysis procedure is
Obtain am and dac copolymer finished product.
In the present invention, described dac monomer with the percentage by weight of am monomer is: the weight of described dac monomer and am monomer
Percentage ratio is: dac monomer 45%, am monomer 55%.
Embodiment two
A kind of am proposed by the present invention and the preparation method of dac copolymer, comprise the following steps:
S1: add acrylyl oxy-ethyl-trimethyl salmiac (dac) monomer in reaction bulb, the reaction outside reaction bulb is filled simultaneously
The temperature put is preset as 5 DEG C, after the temperature of question response device reaches, acrylamide (am) monomer is added with the speed of 1g/min
To in reaction bulb, open agitating device, setting mixing speed is 300r/min, is stirred 10min, obtains mixed solution；
S2: be continually fed into nitrogen 20min in above-mentioned mixed solution, then under conditions of being passed through nitrogen, add in reaction bulb
Enter ammonium sulfate-azodiisobutyronitrile, continue to be stirred with the speed of 300r/min, and observing response during 10～30min
The viscosity of solution and temperature change in device, when reaction temperature begins to decline from maximum temperature, record maximum temperature value, and will be anti-
In answer bottle to be transferred to constant temperature pot that temperature is above-mentioned maximum temperature value, stop being passed through of nitrogen simultaneously, reaction bulb is sealed, goes forward side by side
Row insulation operation 1 hour, reaction bulb is taken out after terminating by insulation operation, naturally cools to 30 DEG C, obtains final product am and dac copolymer
Gel；
S3: the gel of above-mentioned am and dac copolymer is first carried out stripping and slicing, then puts into and carry out pelletize in comminutor, you can obtain
Particle diameter is the gel of the am and dac copolymer of 2mm；
S4: above-mentioned particle diameter is that the gel of the am and dac copolymer of 2mm is dried 5 hours through 50 DEG C and packaging again, and analysis procedure is
Obtain am and dac copolymer finished product.
In the present invention, described dac monomer with the percentage by weight of am monomer is: the weight of described dac monomer and am monomer
Percentage ratio is: dac monomer 80%, am monomer 20%.
Embodiment three
A kind of am proposed by the present invention and the preparation method of dac copolymer, comprise the following steps:
S1: add acrylyl oxy-ethyl-trimethyl salmiac (dac) monomer in reaction bulb, the reaction outside reaction bulb is filled simultaneously
The temperature put is preset as 15 DEG C, after the temperature of question response device reaches, acrylamide (am) monomer is added with the speed of 5g/min
Enter in reaction bulb, open agitating device, setting mixing speed is 200r/min, is stirred 20min, obtains mixed solution；
S2: be continually fed into nitrogen 30min in above-mentioned mixed solution, then under conditions of being passed through nitrogen, add in reaction bulb
Enter ammonium sulfate-azodiisobutyronitrile, continue to be stirred with the speed of 200r/min, and observing response during 10～30min
The viscosity of solution and temperature change in device, when reaction temperature begins to decline from maximum temperature, record maximum temperature value, and will be anti-
In answer bottle to be transferred to constant temperature pot that temperature is above-mentioned maximum temperature value, stop being passed through of nitrogen simultaneously, reaction bulb is sealed, goes forward side by side
Row insulation operation 3 hours, reaction bulb is taken out after terminating by insulation operation, naturally cools to 50 DEG C, obtains final product am and dac copolymer
Gel；
S3: the gel of above-mentioned am and dac copolymer is first carried out stripping and slicing, then puts into and carry out pelletize in comminutor, you can obtain
Particle diameter is the gel of the am and dac copolymer of 1mm；
S4: above-mentioned particle diameter is that the gel of the am and dac copolymer of 1mm is dried 6 hours through 60 DEG C and packaging again, and analysis procedure is
Obtain am and dac copolymer finished product.
In the present invention, described dac monomer with the percentage by weight of am monomer is: the weight of described dac monomer and am monomer
Percentage ratio is: dac monomer 1%, am monomer 90%.
Example IV
A kind of am proposed by the present invention and the preparation method of dac copolymer, comprise the following steps:
S1: add acrylyl oxy-ethyl-trimethyl salmiac (dac) monomer in reaction bulb, the reaction outside reaction bulb is filled simultaneously
The temperature put is preset as 10 DEG C, after the temperature of question response device reaches, acrylamide (am) monomer is added with the speed of 2g/min
Enter in reaction bulb, open agitating device, setting mixing speed is 200r/min, is stirred 20min, obtains mixed solution；
S2: be continually fed into nitrogen 40min in above-mentioned mixed solution, then under conditions of being passed through nitrogen, add in reaction bulb
Enter ammonium sulfate-azodiisobutyronitrile, continue to be stirred with the speed of 200r/min, and observing response during 10～30min
The viscosity of solution and temperature change in device, when reaction temperature begins to decline from maximum temperature, record maximum temperature value, and will be anti-
In answer bottle to be transferred to constant temperature pot that temperature is above-mentioned maximum temperature value, stop being passed through of nitrogen simultaneously, reaction bulb is sealed, goes forward side by side
Row insulation operation 2 hours, reaction bulb is taken out after terminating by insulation operation, naturally cools to 40 DEG C, obtains final product am and dac copolymer
Gel；
S3: the gel of above-mentioned am and dac copolymer is first carried out stripping and slicing, then puts into and carry out pelletize in comminutor, you can obtain
Particle diameter is the gel of the am and dac copolymer of 3mm；
S4: above-mentioned particle diameter is that the gel of the am and dac copolymer of 3mm is dried 3 hours through 40 DEG C and packaging again, and analysis procedure is
Obtain am and dac copolymer finished product.
In the present invention, described dac monomer with the percentage by weight of am monomer is: the weight of described dac monomer and am monomer
Percentage ratio is: dac monomer 50%, am monomer 50%.
With dac copolymer, purity detecting is carried out to the am of embodiment one～tetra- preparation, testing result is as follows:
| Embodiment one | Embodiment two | Embodiment three | Example IV | |
| Purity | 99.3% | 98.6% | 99.2% | 99.6% |
Above-mentioned testing result shows, using the am prepared by preparation method proposed by the present invention and dac copolymer, purity is all relatively
Height, can reach more than 98.6% according to the testing result display purity of embodiment one～tetra-, and result of the test shows that nitrogen leads to
The time length entering can affect the purity of the am and dac copolymer finished product prepared, embodiment four-way in embodiment one～tetra-
The nitrogen time entering is the longest, and the am of its preparation can reach 99.6% with the purity of dac copolymer finished product, and embodiment two is passed through
The nitrogen time the shortest, the am that prepared than example IV with the purity of dac copolymer finished product of am of its preparation is become with dac copolymer
The purity of product is low, but still can reach 98.6%, illustrates that preparation method proposed by the present invention highly purified can obtain am and dac altogether
Polymers.
Flocculating experiment, experiment parameter are carried out to the am and dac copolymer and commercially available flocculant of embodiment one～tetra- preparation
As follows: mixing speed 200r/min, am and dac copolymer consumption are 0.05%, detection flocculation required time, and experimental result is as follows:
| Commercially available flocculant | Embodiment one | Embodiment two | Embodiment three | Example IV | |
| Time | 60s | 25s | 32s | 27s | 21s |
Above-mentioned flocculating experiment result shows, using the am prepared by preparation method proposed by the present invention and dac copolymer, flocculation effect
Really good, flocculation required time is shorter, can reach 21s the soonest according to the experimental result display flocculation time of embodiment one～tetra-,
The most slowly be 32s, all more commercially available flocculant time short.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of am and dac copolymer is it is characterised in that comprise the following steps:
S1: add acrylyl oxy-ethyl-trimethyl salmiac (dac) monomer in reaction bulb, the reaction outside reaction bulb is filled simultaneously
The temperature put is preset as 0～30 DEG C, after the temperature of question response device reaches, by acrylamide (am) monomer with 1～15g/min's
Speed is added in reaction bulb, opens agitating device, and setting mixing speed is 200～300r/min, it is stirred 10～
20min, obtains mixed solution；
S2: be continually fed into nitrogen 20～40min in above-mentioned mixed solution, then under conditions of being passed through nitrogen, to reaction bulb
Middle addition initiator system, continues to be stirred with the speed of 200～300r/min, and observing response device during 10～30min
The viscosity of middle solution and temperature change, when reaction temperature begins to decline from maximum temperature, record maximum temperature value, and will react
Bottle is transferred in the constant temperature pot that temperature is above-mentioned maximum temperature value, stops being passed through of nitrogen simultaneously, reaction bulb is sealed, and carries out
Insulation operation 1～3 hour, reaction bulb is taken out after terminating by insulation operation, naturally cools to 30～50 DEG C, obtains final product am and dac altogether
The gel of polymers；
S3: the gel of above-mentioned am and dac copolymer is first carried out stripping and slicing, then puts into and carry out pelletize in comminutor, you can obtain
Particle diameter is the gel of the am and dac copolymer of 1～3mm；
S4: above-mentioned particle diameter is the gel drying again of the am and dac copolymer of 1～3mm, packaging, and analysis procedure obtains final product am and dac
Copolymer finished product.
2. a kind of am according to claim 1 and dac copolymer preparation method it is characterised in that described dac monomer with
The percentage by weight of am monomer is: dac monomer 5～85%, am monomer 95～15%, and the weight of above-mentioned dac monomer and am monomer
Percentage ratio summation is 100%.
3. the preparation method of a kind of am according to claim 1 and dac copolymer is it is characterised in that described initiator system
For Ammonium persulfate .-azodiisobutyronitrile.
4. the preparation method of a kind of am according to claim 1 and dac copolymer is it is characterised in that described initiator system
Consumption be the 0.2～0.5% of dac monomer and am monomer total amount.
5. the preparation method of a kind of am according to claim 1 and dac copolymer is it is characterised in that in described s4 step
The drying temperature of baking operation is 40～60 DEG C.
6. the preparation method of a kind of am according to claim 1 and dac copolymer is it is characterised in that in described s4 step
The drying time of baking operation is 3～6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610745063.9A CN106349427A (en) | 2016-08-29 | 2016-08-29 | AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610745063.9A CN106349427A (en) | 2016-08-29 | 2016-08-29 | AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method |
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| CN106349427A true CN106349427A (en) | 2017-01-25 |
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| CN201610745063.9A Pending CN106349427A (en) | 2016-08-29 | 2016-08-29 | AM (acrylamide) and DAC (acryloyloxyethyl trimethyl ammonium chloride) copolymer preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108912267A (en) * | 2018-06-11 | 2018-11-30 | 宁夏神耀科技有限责任公司 | The coal gasified black water processing preparation method of cationic polyacrylamide flocculant agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372524A (en) * | 2008-10-17 | 2009-02-25 | 四川通丰科技有限公司 | Process for producing cation polyacrylamide |
| CN101654498A (en) * | 2009-06-30 | 2010-02-24 | 山东宝莫生物化工股份有限公司 | Method for preparing high molecular weight cationic polyacrylamide employing single-initiator |
| CN103570868A (en) * | 2013-10-25 | 2014-02-12 | 安徽循环经济技术工程院 | Aqueous solution polymerization preparation method for (meth)acrylamido propyl trimethyl ammonium chloride and acrylamide copolymer |
-
2016
- 2016-08-29 CN CN201610745063.9A patent/CN106349427A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372524A (en) * | 2008-10-17 | 2009-02-25 | 四川通丰科技有限公司 | Process for producing cation polyacrylamide |
| CN101654498A (en) * | 2009-06-30 | 2010-02-24 | 山东宝莫生物化工股份有限公司 | Method for preparing high molecular weight cationic polyacrylamide employing single-initiator |
| CN103570868A (en) * | 2013-10-25 | 2014-02-12 | 安徽循环经济技术工程院 | Aqueous solution polymerization preparation method for (meth)acrylamido propyl trimethyl ammonium chloride and acrylamide copolymer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108912267A (en) * | 2018-06-11 | 2018-11-30 | 宁夏神耀科技有限责任公司 | The coal gasified black water processing preparation method of cationic polyacrylamide flocculant agent |
| CN108912267B (en) * | 2018-06-11 | 2020-09-29 | 宁夏神耀科技有限责任公司 | Preparation method of cationic polyacrylamide flocculant for coal gasification black water treatment |
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