CN106432599A - Hyperbranched polyacrylamide and preparation method thereof - Google Patents
Hyperbranched polyacrylamide and preparation method thereof Download PDFInfo
- Publication number
- CN106432599A CN106432599A CN201610864755.5A CN201610864755A CN106432599A CN 106432599 A CN106432599 A CN 106432599A CN 201610864755 A CN201610864755 A CN 201610864755A CN 106432599 A CN106432599 A CN 106432599A
- Authority
- CN
- China
- Prior art keywords
- acrylamide
- intermediate product
- hyperbranched poly
- ethyl
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
-
- 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
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses hyperbranched polyacrylamide and a preparation method thereof. A redox initiation system is formed by using ceric ammonium nitrate as an initiator and using pentaerythritol as a branching agent, acrylamide and acryloyloxyethyl trimethyl ammonium chloride or 2-acrylamido-2-methylpropanesulfonic acid are polymerized through free radicals, hydrolysis is conducted through tetraethyl orthosilicate, and then silicon dioxide and hyperbranched polyacrylamide are obtained. The obtained hyperbranched polyacrylamide has the highly branched structure and the unique properties such as the low viscosity, the high rheological property, the good solubility and the molecular interior hole structure, can better treat high-concentration wastewater and has the good flocculation effect.
Description
Technical field
The invention belongs to polystyrene acid amides technical field, it is related to a kind of hyperbranched poly acrylamide；The invention still further relates to
A kind of preparation method of hyperbranched poly acrylamide.
Background technology
Hyperbranched poly acrylamide, compared with traditional linear polypropylene acid amides, has a branched structure of height, low viscosity,
Unique property such as high rheological variation, good dissolubility, intramolecule void structure, is capable of the waste water of higher process high concentration,
There is excellent flocculating effect.Acrylamide, as good organic flocculant, can be divided into cationic, anionic, both sexes
Type polyacrylamide, polyacrylamide can become acrylamide derivative by modified, graft copolymerization.Both sexes acrylamide both had
Have the advantages that anionic property has cationic again, has good water-soluble, very high relative molecular mass and good gluing
Property capacity.Under the conditions of different medium, its carried ionic type may different it is adaptable to process the pollutant of band difference electric charges,
Become the focus of research at present.
Content of the invention
It is an object of the invention to provide a kind of hyperbranched poly acrylamide, this hyperbranched poly acrylamide is with pentaerythrite
For core, there is the branched structure of height, the uniqueness such as low viscosity, high rheological variation, good dissolubility, intramolecule void structure
Property, is capable of the waste water of higher process high concentration, has excellent flocculating effect.
Another object of the present invention is to providing the preparation method of above-mentioned hyperbranched poly acrylamide.
The purpose of the present invention is achieved through the following technical solutions：
With pentaerythrite as core, its structure is shown as this hyperbranched poly acrylamide：
Another technical scheme of the present invention is：The preparation method of above-mentioned hyperbranched poly acrylamide, including using cerous nitrate
As initiator, pentaerythrite, as branching agent, constitutes redox initiation system to ammonium, then passes through radical polymerization acryloyl
Amine, acrylyl oxy-ethyl-trimethyl salmiac or 2- acrylamide-2-methyl propane sulfonic, are being obtained by teos hydrolysis
Silica and hyperbranched poly acrylamide, detailed process comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Acrylamide, deionized water and pentaerythrite are mixed under the protection of nitrogen
Carry out heating water bath, obtain intermediate product a；
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b should be obtained afterwards；
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction；
Step 4, adds tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, use after reaction 2.5-5.5h
Acetone washs and soaks clear viscous liquids, is then dried to obtain hyperbranched poly acrylamide.
Further, the feature of the present invention also resides in：
Acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic wherein in step 1
Mass ratio be 7:2:2、5:2:4、5:4:2、4:6:2 or 4:2:6.
Wherein pentaerythrite and the mass ratio of ceric ammonium nitrate solution are 55:3, the wherein quality of ammonium ceric nitrate is acryloyl
The 0.2-0.4% of amine, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic gross mass.
Wherein deionized water is acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- methyl-prop
The 20% of sulfonic acid gross mass.
Wherein in step 4, the quality of tetraethyl orthosilicate is the 5-11% of acrylamide.
Wherein in step 1, the temperature of heating water bath is 40-70 DEG C, and while heating, reaction solution is stirred,
Heating 10-30min, obtains intermediate product a.
After the dropping ceric ammonium nitrate solution in intermediate product a wherein in step 2, react 10-30min.
Wherein wash and soak clear viscous liquids in step 4 using acetone, soak time is 6h, then in 40 DEG C of constant temperature
Under be dried, obtain white solid, as hyperbranched poly acrylamide.
The invention has the beneficial effects as follows：With ammonium ceric nitrate as initiator, pentaerythrite is branching agent to the present invention, constitutes oxidation
Reduction initiating system, then pass through radical polymerization acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
2- methyl propane sulfonic acid, obtains branched polyacrylamide, then obtains silica by teos hydrolysis and is polymerized
The hyperbranched poly acrylamide arriving.
The hyperbranched poly acrylamide that the present invention obtains, has a branched structure of height, low viscosity, high rheological variation, good
Dissolubility, the unique property such as intramolecule void structure, be capable of the higher waste water processing high concentration, there is excellent flocculation
Effect；And this hyperbranched poly acrylamide high salinity, and good water solubility, and its have simultaneously cation and cloudy from
Some characteristics of sub- flocculant, therefore it has wide range of applications.
Brief description
Fig. 1 is the composition principle figure of the hyperbranched poly acrylamide of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is described in further detail：
The invention provides a kind of hyperbranched poly acrylamide, this hyperbranched poly acrylamide with pentaerythrite as core, its
Chemical structural formula is：
The preparation method of above-mentioned hyperbranched poly acrylamide is：Ammonium ceric nitrate is used as initiator, pentaerythrite conduct
Branching agent, constitutes redox initiation system, then passes through radical polymerization acrylamide, acrylyl oxy-ethyl-trimethyl chlorination
Ammonium or 2- acrylamide-2-methyl propane sulfonic, are obtaining silica and hyperbranched poly acryloyl by teos hydrolysis
Amine, detailed process comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 7:2:2、5:2:4、5:4:2、4:6:2 or 4:2:6；Wherein deionized water be acrylamide,
Acrylyl oxy-ethyl-trimethyl salmiac and the 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite and nitric acid
The mass ratio of cerium ammonium salt solution is 55:3, the wherein quality of ammonium ceric nitrate is acrylamide, acrylyl oxy-ethyl-trimethyl salmiac
0.2-0.4% with 2- acrylamide-2-methyl propane sulfonic gross mass；Acrylamide, deionized water and pentaerythrite are mixed
Get up and carry out heating water bath under the protection of nitrogen, the temperature of heating water bath is 40-70 DEG C, while heating, reaction solution is entered
Row stirring, heats 10-30min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 10-30min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, adds tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, use after reaction 2.5-5.5h
Acetone washs and soaks clear viscous liquids, soaks 6h, is then dried to obtain white solid in the environment of 40 DEG C of constant temperature, as
Hyperbranched poly acrylamide.
The course of reaction of hyperbranched poly acrylamide of the present invention is as shown in figure 1, first using ammonium ceric nitrate as initiator, season penta
Tetrol as branching agent, constitutes redox system, then by with free radical acrylamide (AM), acrylyl oxy-ethyl front three
Ammonium chloride (DAC) and the polymerization of 2- acrylamide-2-methyl propane sulfonic (AMPS), obtain branched polyacrylamide；Branched poly-
Propylene milling amine is reacted with tetraethyl orthosilicate, is hydrolyzed into the hyperbranched poly acrylamide that silica and in-situ polymerization become.
Wherein reactant silica is easily processed, and is easy to the purification of hyperbranched poly acrylamide.
The embodiment that the present invention prepares hyperbranched poly acrylamide includes：
Embodiment 1
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 7:2:2；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.2% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 40 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 10min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 10min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, adds tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, using acetone after reaction 2.5h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white in the environment of 40 DEG C of constant temperature using drying box solid
Body, as hyperbranched poly acrylamide.
Embodiment 2
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 5:2:4；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.3% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 50 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 20min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 20min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, is added tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, washed using acetone after reaction 3h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white solid using drying box in the environment of 40 DEG C of constant temperature,
It is hyperbranched poly acrylamide.
Embodiment 3
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 5:4:2；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.4% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 60 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 30min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 30min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, is added tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, washed using acetone after reaction 4h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white solid using drying box in the environment of 40 DEG C of constant temperature,
It is hyperbranched poly acrylamide.
Embodiment 4
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 4:6:2；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.35% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 70 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 25min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 25min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, adds tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, using acetone after reaction 5.5h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white in the environment of 40 DEG C of constant temperature using drying box solid
Body, as hyperbranched poly acrylamide.
Embodiment 5
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 4:2:6；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.25% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 45 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 15min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 15min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, adds tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, using acetone after reaction 4.5h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white in the environment of 40 DEG C of constant temperature using drying box solid
Body, as hyperbranched poly acrylamide.
Embodiment 6
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 7:2:2；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.4% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 70 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 24min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 25min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, is added tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, washed using acetone after reaction 3h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white solid using drying box in the environment of 40 DEG C of constant temperature,
It is hyperbranched poly acrylamide.
Embodiment 7
A kind of preparation detailed process of present invention hyperbranched poly acrylamide comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, goes
Ionized water, pentaerythrite and ammonium ceric nitrate；Wherein acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-
The mass ratio of 2- methyl propane sulfonic acid is 5:2:4；Wherein deionized water be acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and
The 20% of 2- acrylamide-2-methyl propane sulfonic gross mass；Pentaerythrite is 55 with the mass ratio of ceric ammonium nitrate solution:3, wherein
The quality of ammonium ceric nitrate is that acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic are total
The 0.4% of quality；Acrylamide, deionized water and pentaerythrite are mixed and is placed on heating water bath in there-necked flask, water
The temperature of bath heating is 60 DEG C, and wherein there-necked flask a mouth is used for being passed through shielding gas nitrogen, and a mouth is used for stirring, one
Mouth is discharged for gas；Heating 18min, obtains intermediate product a.
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, instead in intermediate product a
Intermediate product b is obtained after answering 18min.
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- first in intermediate product b
Base propane sulfonic acid, obtains intermediate product c after reaction.
Step 4, is added tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, washed using acetone after reaction 4h
Wash and soak clear viscous liquids, soak 6h, be then dried to obtain white solid using drying box in the environment of 40 DEG C of constant temperature,
It is hyperbranched poly acrylamide.
Claims (9)
1. a kind of hyperbranched poly acrylamide is it is characterised in that this hyperbranched poly acrylamide is with pentaerythrite as core, its structure
It is shown as：
2. a kind of preparation method of hyperbranched poly acrylamide is it is characterised in that include ammonium ceric nitrate being used as initiator, season
Penta tetrol, as branching agent, constitutes redox initiation system, then passes through radical polymerization acrylamide, acrylyl oxy-ethyl
Trimethyl ammonium chloride or 2- acrylamide-2-methyl propane sulfonic, are obtaining silica and over-expense by teos hydrolysis
Change polyacrylamide, detailed process comprises the following steps：
Step 1, takes acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, 2- acrylamide-2-methyl propane sulfonic, deionization
Water, pentaerythrite and ammonium ceric nitrate；Acrylamide, deionized water and pentaerythrite are mixed and carries out under the protection of nitrogen
Heating water bath, obtains intermediate product a；
Step 2, drips initiator ceric ammonium nitrate solution, the concentration of ceric ammonium nitrate solution is 1%, reacts it in intermediate product a
After obtain intermediate product b；
Step 3, sequentially adds acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide -2- methyl-prop in intermediate product b
Sulfonic acid, obtains intermediate product c after reaction；
Step 4, adds tetraethyl orthosilicate in intermediate product c, obtains clear viscous liquids, using acetone after reaction 2.5-5.5h
Wash and soak clear viscous liquids, be then dried to obtain hyperbranched poly acrylamide.
3. the preparation method of hyperbranched poly acrylamide according to claim 2 is it is characterised in that third in described step 1
The mass ratio of acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic is 7:2:2、5:2:
4、5:4:2、4:6:2 or 4:2:6.
4. hyperbranched poly acrylamide according to claim 3 preparation method it is characterised in that described pentaerythrite with
The mass ratio of ceric ammonium nitrate solution is 55:3, the wherein quality of ammonium ceric nitrate is acrylamide, acrylyl oxy-ethyl-trimethyl chlorine
Change the 0.2-0.4% of ammonium and 2- acrylamide-2-methyl propane sulfonic gross mass.
5. the preparation method of hyperbranched poly acrylamide according to claim 3 is it is characterised in that described deionized water is
The 20% of acrylamide, acrylyl oxy-ethyl-trimethyl salmiac and 2- acrylamide-2-methyl propane sulfonic gross mass.
6. the preparation method of hyperbranched poly acrylamide according to claim 3 is it is characterised in that in described step 4 just
The quality of silester is the 5-11% of acrylamide.
7. the preparation method of the hyperbranched poly acrylamide according to claim 2-6 any one is it is characterised in that described
In step 1, the temperature of heating water bath is 40-70 DEG C, and while heating, reaction solution is stirred, and heats 10-30min,
Obtain intermediate product a.
8. the preparation method of the hyperbranched poly acrylamide according to claim 2-6 any one is it is characterised in that described
After the dropping ceric ammonium nitrate solution in intermediate product a in step 2, react 10-30min.
9. the preparation method of the hyperbranched poly acrylamide according to claim 2-6 any one is it is characterised in that described
Wash and soak clear viscous liquids in step 4 using acetone, soak time is 6h, is then dried under 40 DEG C of constant temperature,
Obtain white solid, as hyperbranched poly acrylamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610864755.5A CN106432599A (en) | 2016-09-29 | 2016-09-29 | Hyperbranched polyacrylamide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610864755.5A CN106432599A (en) | 2016-09-29 | 2016-09-29 | Hyperbranched polyacrylamide and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106432599A true CN106432599A (en) | 2017-02-22 |
Family
ID=58169953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610864755.5A Pending CN106432599A (en) | 2016-09-29 | 2016-09-29 | Hyperbranched polyacrylamide and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106432599A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107118301A (en) * | 2017-03-24 | 2017-09-01 | 陕西科技大学 | A kind of hyperbranched amphiprotic polyacrylamide and preparation method thereof |
| CN107602764A (en) * | 2017-09-17 | 2018-01-19 | 杨文思 | A kind of new hyperbranched copolymer ceramics reinforcing agent and preparation method and application |
| CN108003284A (en) * | 2017-11-21 | 2018-05-08 | 陕西科技大学 | A kind of hyperbranched cationic polyacrylamide and preparation method thereof |
| CN108786415A (en) * | 2018-05-29 | 2018-11-13 | 安徽省银锂子生物科技发展有限公司 | A kind of environmentally protective sterilization methanal scavenger |
| CN110054725A (en) * | 2019-04-19 | 2019-07-26 | 常州大学 | A kind of polymerizable single active center's redox initiation system of hydrolysis |
| CN115584633A (en) * | 2022-09-23 | 2023-01-10 | 冯亚斌 | Household waterproof oil-resistant polyethylene fabric and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070298006A1 (en) * | 2004-04-20 | 2007-12-27 | Dendritic Nanotechnologies, Inc. | Dendritic Polymers With Enhanced Amplification and Interior Functionality |
| CN104844765A (en) * | 2015-05-18 | 2015-08-19 | 中国海洋石油总公司 | Hyperbranched polymer oil-displacing agent and preparation method thereof |
-
2016
- 2016-09-29 CN CN201610864755.5A patent/CN106432599A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070298006A1 (en) * | 2004-04-20 | 2007-12-27 | Dendritic Nanotechnologies, Inc. | Dendritic Polymers With Enhanced Amplification and Interior Functionality |
| CN104844765A (en) * | 2015-05-18 | 2015-08-19 | 中国海洋石油总公司 | Hyperbranched polymer oil-displacing agent and preparation method thereof |
Non-Patent Citations (7)
| Title |
|---|
| WANFEN PU，ET AL: "Synthesis and characterization of hyperbranched associative polyacrylamide", 《REC ADV.》 * |
| WAN-FEN PU，ET AL: "Water-Soluble Core-Shell Hyperbranched Polymers for Enhanced Oil Recovery", 《IND.ENG.RES.》 * |
| 丛珊: "超支化阳离子聚丙烯酰胺的制备及应用研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 张昊等: "阳离子型超支化聚丙烯酰胺的合成与反应中影响产物黏度因素的探讨", 《当代化工》 * |
| 朱阳阳等: "两性聚丙烯酰胺的性质、合成与应用研究进展", 《化工进展》 * |
| 柳蝉等: "星形阴离子型聚丙烯酰胺的合成及絮凝性能", 《烟台大学学报（自然科学与工程版）》 * |
| 程建华等: "P(AM/AMPS/DAC)两性型絮凝剂的制备与应用", 《中国环境科学学会学术年会论文集（2009）》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107118301A (en) * | 2017-03-24 | 2017-09-01 | 陕西科技大学 | A kind of hyperbranched amphiprotic polyacrylamide and preparation method thereof |
| CN107602764A (en) * | 2017-09-17 | 2018-01-19 | 杨文思 | A kind of new hyperbranched copolymer ceramics reinforcing agent and preparation method and application |
| CN108003284A (en) * | 2017-11-21 | 2018-05-08 | 陕西科技大学 | A kind of hyperbranched cationic polyacrylamide and preparation method thereof |
| CN108786415A (en) * | 2018-05-29 | 2018-11-13 | 安徽省银锂子生物科技发展有限公司 | A kind of environmentally protective sterilization methanal scavenger |
| CN108786415B (en) * | 2018-05-29 | 2020-07-17 | 安徽省银锂子生物科技发展有限公司 | Green and environment-friendly sterilizing formaldehyde scavenger |
| CN110054725A (en) * | 2019-04-19 | 2019-07-26 | 常州大学 | A kind of polymerizable single active center's redox initiation system of hydrolysis |
| CN115584633A (en) * | 2022-09-23 | 2023-01-10 | 冯亚斌 | Household waterproof oil-resistant polyethylene fabric and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106432599A (en) | Hyperbranched polyacrylamide and preparation method thereof | |
| Yeap et al. | Preparation and characterization of coagulation/flocculation behavior of a novel inorganic–organic hybrid polymer for reactive and disperse dyes removal | |
| CN103351047B (en) | Organic-inorganic hybrid flocculant and preparation method thereof | |
| Tang et al. | The role of sulfonated chitosan-based flocculant in the treatment of hematite wastewater containing heavy metals | |
| US10443192B2 (en) | Powdery water-soluble cationic polymer composition | |
| Xu et al. | Effect of acid medium on the coagulation efficiency of polysilicate-ferric (PSF)—A new kind of inorganic polymer coagulant | |
| Sun et al. | Comparison of initiation methods in the structure of CPAM and sludge flocs properties | |
| Noppakundilograt et al. | Synthesis of acrylamide/acrylic acid‐based aluminum flocculant for dye reduction and textile wastewater treatment | |
| Guan et al. | Preparation, characterization, and flocculation performance of P (acrylamide‐co‐diallyldimethylammonium chloride) by UV‐initiated template polymerization | |
| CN102557218A (en) | Composite flocculating agent containing various polyacrylamides and preparation method for composite flocculating agent | |
| CN104448082B (en) | A kind of calcium ions modified polyacrylamide preparation method | |
| Liu et al. | Synthesis of a novel amphoteric chelating polymer flocculant and its performance in Cu2+ removal | |
| Chen et al. | Characterization and flocculation evaluation of a new organic–inorganic hybrid polymer flocculant (PAC‐AM‐DMC) | |
| Sun et al. | Synthesis of a cationic polyacrylamide under UV initiation and its flocculation in estrone removal | |
| Abdiyev et al. | Flocculating properties of 2-acrylamido-2-methyl-1-propane sulfonic acid-co-allylamine polyampholytic copolymers | |
| CN101921015A (en) | Novel inorganic-organic composite macromolecular decolorizing flocculant and preparation method thereof | |
| CN103304016B (en) | A kind of method utilizing attapulgite to prepare hybrid flocculant | |
| CN107118301A (en) | A kind of hyperbranched amphiprotic polyacrylamide and preparation method thereof | |
| CN110282715B (en) | Preparation and application of polyquaternium in-situ composite modified polymeric ferric sulfate | |
| CN108003284A (en) | A kind of hyperbranched cationic polyacrylamide and preparation method thereof | |
| CN103395870B (en) | Preparation method of composite flocculant | |
| JPH0338204A (en) | Treating technique for low concentration turbid water | |
| CN104356268B (en) | A kind of preparation method of modified polyacrylamide containing magnesium ion | |
| CN110040831B (en) | Preparation method of sodium alginate-polymethacryloxyethyl trimethyl ammonium chloride organic flocculant | |
| Bouras et al. | Optimizing the coagulation/flocculation process for bentonite suspension with poly (acrylamide-co-(N-methyl-4-vinylpyridinium tosylate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170222 |
|
| RJ01 | Rejection of invention patent application after publication |