Preparation method of high-branching retardation type polycarboxylic acid water reducing agent
A technology of retarded polycarboxylate and high branching, applied in the field of retarded polycarboxylate superplasticizers, can solve the problems of high mud content and failure to meet the requirements, and achieve excellent dispersion effect, simple method, The effect of improving reaction efficiency
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Embodiment 1
[0025] 1) Preparation of high-branched copolymerization products containing azido groups: 10mol hydroxymethyl acrylate, 10mol p-chloromethylstyrene and 0.01mol CuBr / pentamethyldiethylenetriamine (PMDETA) (wherein CuBr and PMDETA The molar ratio is 1:1) through redox reaction to carry out atom transfer radical polymerization (ATRP) reaction for 30min, add 10.1mol sodium azide and stir for 30min, after desalination, obtain molecular weight 3000 and branching degree 10 containing azide Nitrogen-based highly branched copolymerization product;
[0026] 2) Preparation of alkynyl polyethylene glycol monomethyl ether: gradually add 10.1 mol of sodium hydride powder to 10 mol of polyethylene glycol monomethyl ether with a molecular weight of 400 at 10°C, and add a certain amount of 10.1 mol after reacting at room temperature for 30 minutes Propylene bromide, then stirred and reacted for 30min to obtain alkynyl polyethylene glycol monomethyl ether after desalination;
[0027] 3) Prepar...
Embodiment 2
[0029] 1) Preparation of high-branched copolymerization products containing azido groups: 10mol hydroxyethyl acrylate, 1mol p-bromomethylstyrene and 0.11mol CuCl / HMTETA (the molar ratio of CuCl to HMTETA is 1:2) were passed through Oxidation-reduction reaction carries out atom transfer radical polymerization (ATRP) reaction 35min, adds 11mol sodium azide in stirring reaction 40min, after desalting, obtain molecular weight and be 3500 and branch degree be 14 to contain the azide group highly branched copolymerization product;
[0030] 2) Preparation of alkynyl polyethylene glycol monomethyl ether: gradually add 11 mol of sodium hydride powder to 10 mol of polyethylene glycol monomethyl ether with a molecular weight of 500 at 20°C, and add a certain amount of 11 mol of propyne after reacting at room temperature for 30 minutes Bromine, then stirred and reacted for 40min to obtain alkynyl polyethylene glycol monomethyl ether after desalination
[0031] 3) Preparation of high-branc...
Embodiment 3
[0033] 1) Preparation of high-branched copolymerization products containing azido groups: 10mol hydroxy-n-butyl acrylate, 8mol chloromethylated polystyrene resin (CMPS) and 0.2mol CuBr / tetrakis[(2-pyridyl)methyl Base] Ethylenediamine (TPEN) (the molar ratio of CuBr to TPEN is 1:2) undergoes atom transfer radical polymerization (ATRP) reaction by redox reaction for 40min, adds 11mol sodium azide and stirs for 120min, after desalination The obtained molecular weight is 5000 and the degree of branching is 20 containing the azide group hyperbranched copolymerization product;
[0034]2) Preparation of alkynyl polyethylene glycol monomethyl ether: gradually add 10.5 mol of sodium hydride powder to 10 mol of polyethylene glycol monomethyl ether with a molecular weight of 800 at 35°C, and add a certain amount of 11 mol of propyne after reacting at room temperature for 30 minutes bromine, then stirred and reacted for 50min to obtain alkynyl polyethylene glycol monomethyl ether after de...
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