Alkenyl acid chloride alcoholysis to prepare the method of macromonomer synthesis polycarboxylate water reducing agent

A technology for synthesizing polycarboxylic acid and alkenyl chlorohydrin, which is applied in the field of polycarboxylic acid high-performance water reducer for concrete, can solve the problems of failure to achieve functional regulation of chemical admixtures, limit popularization and application, and achieve extreme side effects , expanding the theoretical connotation, and the effect of mild and stable polymerization reaction process

CN106117461BActive Publication Date: 2018-03-30BEIJING UNIV OF TECH
3 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2018-03-30

Smart Images

  • Figure 1
    Figure 1
  • Figure 2
    Figure 2
  • Figure 3
    Figure 3
Patent Text Reader

Abstract

A method for preparing a macro-monomer synthesized polycarboxylate water reducer through alcoholysis of alkenyl-acyl chloride belongs to the field of water reducers. The method comprises the following steps: firstly polymerizing a cationic chain, and then reacting with the alkenyl-acyl chloride, thus obtaining a macro-monomer; then carrying out copolymerization on the macro-monomer and a carboxylic acid micro-monomer, i.e., polymerizing under an oxidization-reduction initiating system formed by high-valence cerate and alcohols by taking an unsaturated cationic quaternary ammonium salt monomer as a reactant, thus obtaining a terminal hydroxyl cationic long chain; then respectively enabling the terminal hydroxyl cationic long chain and polyethylene glycol monomothyl ether to react with the alkenyl-acyl chloride respectively, thus preparing macro-monomers with different structures; then carrying out free radical polymerization on the macro-monomers and unsaturated carboxylic acid micro-monomers, thus obtaining the macro-monomer composite polycarboxylate water reducer. According to the method disclosed by the invention, the macro-monomers with different structures and functions are successfully synthesized through ways of polymerizing the cationic chain and respectively reacting with the alkenyl-acyl chloride by combining polyether, and a novel comb-structure polycarboxylate water reducer which takes a polycarboxyl acid as a main chain and the cationic long chain and the polyether as polybasic side chains can be finally obtained. A reaction technology is simple and easy, and multiple excellent effects of retaining slump through reducing water, resisting clay, and the like are realized.
Need to check novelty before this filing date? Find Prior Art

Description

technical field

[0001] The invention relates to the technical field of a polycarboxylic acid high-performance water reducer for concrete, in particular to a polycarboxylate high-performance water reducer that uses an unsaturated cationic quaternary ammonium salt to first polymerize and then react with alkenyl acid chloride to form a macromonomer and then react with unsaturated carboxylic acid to form a small monomer. The specific preparation method of monomer copolymerization into polycarboxylate water reducer. Background technique

[0002] Because it can prevent the loss of concrete slump without causing obvious retardation, it can exert a high plasticizing effect at low dosage, and has good fluidity retention, large room for high performance, high degree of freedom in molecular structure, and good for concrete. Remarkable strengthening and shrinkage reduction effects, extremely low content of harmful substances and other technical performance characteristics, polycarboxyla...

Examples

Embodiment 1

[0027] First, 22.07g of methacryloylpropyltrimethylammonium chloride and 1g of cyclohexanol were added to the reactor, and then 553.81g of water was added to prepare an aqueous solution with a mass concentration of 4%, and the reactor was filled with nitrogen to remove oxygen repeatedly 3 times Seal it after 18 minutes, add 5.97g of ceric ammonium sulfate, stir for 18 minutes until it is mixed evenly, continue to heat up to 10°C for polymerization reaction, and react for 16 hours to obtain an aqueous solution of hydroxyl-terminated cation side chains; The aqueous solution was vacuumed to remove the water in the system, and 25g of polyethylene glycol monomethyl ether (molecular weight=500), 5.43g of acryloyl chloride, and 262.52g of dimethylformamide were sequentially added, and the stirring time was 10 minutes between each addition, and the temperature was raised to 40 ℃, after 4 hours of reaction, add 420.03g of methanol, wash the precipitate repeatedly 5 times, vacuum dry the...

Embodiment 2

[0029] After the polycarboxylate superplasticizer solution with a mass fraction of 30% obtained in Example 1 was stored at 6° C. for 20 days, its implementation effect was measured.

Embodiment 3

[0031] First, 14.71g of methacryloyloxyethyl dimethyl butyl ammonium bromide and 0.74g of isobutanol were added to the reactor, then 757.11g of water was added to prepare an aqueous solution with a mass concentration of 2%, and the reactor was filled with nitrogen repeatedly After 4 times of deoxygenation for 30 minutes, seal it, add 0.6g of ammonium cerium sulfate, stir for 30 minutes until it is evenly mixed, continue to heat up to 55°C for polymerization reaction, and react for 6 hours to obtain an aqueous solution of hydroxyl-terminated cation side chains; The hydroxyl cation side chain aqueous solution was vacuumed to remove the water in the system, and 45g polyethylene glycol monomethyl ether (molecular weight = 3000), 3.66g methacryloyl chloride, 253.47g dimethyl sulfoxide were added in sequence, and the stirring time between each addition was After 12 minutes, the temperature was raised to 85°C. After 2.5 hours of reaction, 633.69g of methanol was added, the precipitate...