Preparation method of series cationic degree and high intrinsic viscosity p(dac-am)

A cationic degree and characteristic viscosity technology, which is applied in the field of preparation of cationic polyacrylamide copolymers, can solve problems such as continuous decline in monomer content, limited characteristic viscosity of polymerization products, incomplete cationic degree coverage, etc., to prevent characteristic viscosity. Loss, improved monomer conversion, and easy drying effects

Active Publication Date: 2021-06-08
NANJING UNIV OF SCI & TECH
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Problems solved by technology

However, the two-step heating method cannot overcome the shortage that the monomer content in the system continues to decrease as the reaction progresses, and the further increase of the intrinsic viscosity is limited.
[0011] It can be seen from the above that the synthesis process of P(DAC-AM) has changed from one-step heating method to two-step heating method, which has fully played the role of initiator and improved the intrinsic viscosity and monomer conversion rate of colloidal products; however, it cannot To overcome the shortage of the continuous decrease of the monomer content in the system, which limits the further increase of the intrinsic viscosity of the polymerization product
In addition, due to the limitation of the level of process research, the cation degree of the synthesized P(DAC-AM) is not fully covered.

Method used

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  • Preparation method of series cationic degree and high intrinsic viscosity p(dac-am)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The first step, in the polymerization reactor that has thermometer, stirrer, condensing recovery steam and nitrogen device, add the mixed solution that mass ratio is the methanol and ethanol of 80:20, get the content of alcohol (in mass fraction, below The same) is (5.00±0.01)% alcohol aqueous solution, then add industrial monomers DAC and AM with a substance ratio of 1:9, add alcohol water to adjust the monomer content of the system to 20%, and stir evenly under nitrogen atmosphere ;

[0031] In the second step, in the above-mentioned reaction kettle, the metal complexing agent tetrasodium ethylenediamine tetraacetate of 0.035% by mass ratio of the monomers is added, and the molar ratio of ammonium persulfate and sodium bisulfite is 2:1, accounting for The monomer mass ratio is 0.57%;

[0032] In the third step, nitrogen gas is introduced, and after stirring for 20 minutes, the reaction liquid is heated to (32.0±1.0)°C, and the heat preservation polymerization is carr...

Embodiment 2

[0036] In the first step, a mixture of methanol and ethanol with a mass ratio of 40:60 is added to a polymerization reactor equipped with a thermometer, a stirrer, steam condensation recovery and a nitrogen device to obtain an alcohol content of (3.00 ± 0.01)% Alcohol aqueous solution, then add industrial monomers DAC and AM with a substance ratio of 3:7, add alcohol water to adjust the monomer content of the system to 37%, and stir evenly under a nitrogen atmosphere;

[0037] In the second step, in the above-mentioned reaction kettle, the metal complexing agent tetrasodium ethylenediamine tetraacetate of 0.030% by mass ratio of the monomers is added, and the molar ratio of ammonium persulfate and sodium bisulfite is 2:1, accounting for The monomer mass ratio is 0.36%;

[0038] In the third step, nitrogen gas is introduced, and after stirring for 20 minutes, the reaction solution is heated to (35.0±1.0)°C, and the temperature is maintained for (3.0±0.5) hours;

[0039] The fo...

Embodiment 3

[0042] In the first step, a mixed solution of methanol and ethanol with a mass ratio of 20:80 is added to a polymerization reactor with a thermometer, a stirrer, steam condensation recovery and a nitrogen device to obtain an alcohol content of (1.00 ± 0.01)%. Alcohol aqueous solution, then add industrial monomers DAC and AM with a substance ratio of 5:5, add alcohol water to adjust the monomer content of the system to 40%, and stir evenly under a nitrogen atmosphere;

[0043] In the second step, in the above-mentioned reaction kettle, the metal complexing agent tetrasodium ethylenediamine tetraacetate of 0.025% by mass ratio of the monomers is added, and the molar ratio of ammonium persulfate and sodium bisulfite is 1:1, accounting for The monomer mass ratio is 0.27%;

[0044] In the third step, nitrogen gas is introduced, and after stirring for 20 minutes, the reaction solution is heated to (38.0±1.0)°C, and the polymerization is carried out for (3.0±0.5) hours;

[0045] The...

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Abstract

The invention discloses a preparation method of P(DAC‑AM) with serial cationicity and high intrinsic viscosity. The method uses industrial monomers DAC and AM as raw materials, uses a redox initiator, and an alcohol-containing aqueous solution polymerization method. According to different cationic degrees, the temperature-programmed initiation and thermal insulation polymerization conditions are selected, and the polymerization is initiated step by step, and synchronously removed and recovered. Alcohol solvent step to obtain P(DAC‑AM) colloidal product, the colloid is granulated and dried to obtain P(DAC‑AM) easily soluble dry powder with serial cationicity, high intrinsic viscosity and high monomer conversion rate. The P(DAC-AM) dry powder prepared by the invention has a cationic degree of 10%-90%, an intrinsic viscosity of 15.12-26.30dL / g, and a monomer conversion rate of over 99.50%.

Description

technical field [0001] The invention belongs to the technical field of preparation of cationic polyacrylamide copolymers, and relates to a preparation method of serialized cationic degree and high intrinsic viscosity P(DAC-AM). Background technique [0002] Cationic polyacrylamide P (DAC-AM) (formula 1) is a copolymer of acryloyloxyethyltrimethyl ammonium chloride (DAC for short) and acrylamide (AM for short), and is a A commonly used organic cationic water-soluble polymer. Because of its adjustable cationic degree (that is, the molar fraction of the initial DAC in the total monomer) and the viscosity-average relative molecular mass (expressed by the characteristic viscosity [η]), it is widely used in various industrial production fields, especially as a flocculant Used for flocculation and dehydration of printing and dyeing, papermaking and municipal wastewater sludge, it has become one of the most widely used cationic polyacrylamides at home and abroad. [0003] [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/56C08F220/34C08J9/28C08L33/26C08L33/14
Inventor 张跃军陈婷婷
Owner NANJING UNIV OF SCI & TECH
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