Synthetic method of side-chain adsorption type concrete super-plasticizer
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A superplasticizer, adsorption-type technology, applied in the field of superplasticizer for cement concrete, can solve the problems of difficult structure innovation and performance optimization, few anionic side chain macromonomers, and limited promotion and application, and achieve excellent Development prospects and application value, inhibition of clay side effects, rich and diverse effects
Active Publication Date: 2019-07-02
BEIJING UNIV OF TECH
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However, the above-mentioned synthesis methods all have certain deficiencies. Researchers mostly focus on achieving water-reducing dispersion, anti-mud, flocculation and other properties through modification and modification, but seldom use controllable polymerization methods to innovate and synthesize anionic side chains. Macromonomer, and based on this synthetic side chain adsorption type concrete superplasticizer, it is difficult to truly expand structural innovation and performance optimization
Only simple main chain or polyether side chain modification limits its application in the field of concrete superplasticizers
Therefore, this requires concrete superplasticizers to achieve fundamental innovations in molecular structure. They must not only have working properties such as water reduction and slump protection, but also have resistance to external environmental influences such as mud resistance. Simple, low cost, abundant and extensive raw materials are also the guarantee for industrialized production and large-scale promotion and application. There are no reports on this aspect at home and abroad.
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Embodiment 1
[0026] First, add 5.05g of acrylic acid, 30.27g of water, and 63.11g of ethylamine into the reactor and mix well, then add 1.79g of ethyl 2-bromoacrylate, 3.8g of ferrous chloride, 10.37g of 1,1,4,7,10,10 - Hexamethyltriethylenetetramine, the reactor was filled with nitrogen in an ice-water bath and deoxygenated repeatedly 5 times for 25 minutes, then stirred for 15 minutes until it was mixed evenly, sealed under nitrogen protection, and continued to heat up to 70°C for polymerization reaction. After 20 hours, the unsaturated macromonomer was obtained after desalting and vacuum distillation to remove the solvent; the obtained unsaturated macromonomer was mixed with 32.4 g of water, the temperature was raised to 60 ° C, and 2.56 g of HCl aqueous solution with a mass fraction of 20% was added, Hydrolyze for 50 minutes, after the hydrolysis is completed, distill under reduced pressure to remove water and by-products to obtain anionic macromonomer; finally dissolve the anionic macr...
Embodiment 2
[0028] After the 30% side chain adsorption concrete superplasticizer solution obtained in Example 1 was stored at 5° C. for 30 days, its implementation effect was measured.
Embodiment 3
[0030] First, 200.22g of ethyl acrylate and 400.44g of dimethylformamide were added to the reactor and mixed evenly, then 1.49g of 1-bromo-3-methyl-2-butene, 1.44g of cuprous bromide, 2.6g of N,N ,N,N,N-Pentamethyldivinyltriamine, the reactor was filled with nitrogen in an ice-water bath and deoxygenated 3 times for 15 minutes, then stirred for 30 minutes until it was evenly mixed, sealed under nitrogen protection and continued to heat up to 10°C Polymerization reaction was carried out at 90°C for 48 hours, desalination and vacuum distillation to remove the solvent to obtain the unsaturated macromonomer; the obtained unsaturated macromonomer was mixed with 161.37g of water, the temperature was raised to 90°C, and 8g was added with a mass fraction of 30 % sodium hydroxide aqueous solution, hydrolyzed for 10 minutes, after the hydrolysis was completed, decompression distillation sloughed water and by-products to obtain anionic macromonomer; finally anionic macromonomer was dissol...
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Abstract
The invention relates to a synthetic method of a side-chain adsorption type concrete super-plasticizer. By using an unsaturated monomer, an unsaturated initiator, a transition metal complex, a carboxylic small monomer and the like as main raw materials and through the method of auto-polymerization, hydrolysis and graft copolymerization, the side-chain adsorption type concrete super-plasticizer issynthesized. The synthetic method specifically comprises the following steps: the unsaturated monomer, which is used as a reactant, is subjected to atom transfer radical polymerization (ATRP) in an initiating system composed of the unsaturated initiator, transition metal halide and a ligand so as to obtain an unsaturated macromonomer; then, the macromonomer is subjected to hydrolysis to obtain ananionic macromonomer; and the anionic macromonomer and the carboxylic small monomer are subjected to radical graft copolymerization under the action of an initiator and a chain transfer agent to prepare the side-chain adsorption type concrete super-plasticizer. The synthetic method of the invention has controllable process and simple step, is convenient and efficient, and is energy-saving and environmentally-friendly. Through innovative design of the molecular structure, the side-chain adsorption type concrete super-plasticizer is synthesized, multiple excellent effects of water reduction andslump retaining and the effect of inhibiting side effect of clay are realized, and the types of the concrete super-plasticizer are enriched.
Description
technical field [0001] The invention relates to the technical field of a superplasticizer for cement concrete, in particular to a superplasticizer that uses unsaturated monomers to self-polymerize and then hydrolyze to form anionic macromonomers, and then graft copolymerizes with carboxylic acid small monomers to form side plasticizers. The specific preparation method of the chain adsorption type concrete superplasticizer. Background technique [0002] The deepening of urbanization and the rapid expansion of infrastructure have led to the rapid development of the construction industry. The amount of concrete and cement is increasing. As one of the important components of concrete, superplasticizers have become a hot spot in concrete research and development. The emergence of polycarboxylate superplasticizers with low dosage, high water-reducing rate and good slump retention has solved the problems of low water-reducing rate and retarded setting of ordinary lignosulfonate-bas...
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