A polycarboxylate concrete high-efficiency water reducer with amide/imide structure and its preparation method
A high-efficiency water reducer and polycarboxylic acid technology, applied in the field of concrete admixtures, can solve the problems of difficult synthesis process, harsh conditions, and many side reactions, and achieve the effects of low cost, energy saving, and good adaptability
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Embodiment 1
[0064] Step 1) Neutralize 45g of ethylamine with equimolar acetic acid and add 107.8g of maleic anhydride into the reactor. Under the protection of nitrogen, heat up to 60°C, add 0.18g of concentrated sulfuric acid, continue to heat up to 95°C, and keep the temperature for 4h , cooling to obtain the acylated product c.
[0065] Step 2) In the glass reactor equipped with thermometer, stirrer, dropping funnel and nitrogen inlet tube, add 200g deionized water, add 12.5g acylate product c, 240g methallyl polyethylene glycol ether simultaneously (Mn=2400g / mol), 19.6g of maleic anhydride, while stirring, purging the reaction vessel with nitrogen, and heating up to 60°C to dissolve, then adding 2.72g of ammonium persulfate, and stirring evenly. Then mix 4.08g of mercaptoacetic acid and 134g of water, stir to form a uniform monomer aqueous solution, add it dropwise to the reactor for 2 hours, keep it warm for 2 hours after the addition, cool to room temperature, and add alkali to neut...
Embodiment 2
[0067] Step 1) After neutralizing 59.1g of N-ethylmethylamine with equimolar acetic acid and adding 168.3g of itaconic anhydride into the reactor, under the protection of nitrogen, the temperature was raised to 60°C, and 0.35g of p-toluenesulfonic acid was added, Continue to raise the temperature to 100°C, keep the temperature constant for 3h, then lower the temperature to obtain the acylated product c.
[0068] Step 2) In the glass reactor equipped with thermometer, stirrer, dropping funnel and nitrogen inlet tube, add 75g of deionized water, add 15.3g of acylated product c, 16.8g of itaconic anhydride at the same time, and use nitrogen gas while stirring Purging reaction vessel, and be warming up to 70 ℃ and dissolve, add dropwise the initiator solution of 200g polyethylene glycol monomethyl ether methacrylate (Mn=2000g / mol) solution, 4.75g sodium persulfate (60g) water and 5.23g of sodium bisulfite, 60g of aqueous solution, the dropping time is 3h, after the dropping is com...
Embodiment 3
[0070] Step 1) After neutralizing 45g of ethylamine with equimolar acetic acid, add 117.6g of maleic anhydride into the reactor, under the protection of nitrogen, heat up to 60°C, add 0.25g of p-toluenesulfonic acid, continue to heat up to 105°C, Keep the temperature for 5 hours, then lower the temperature to obtain the acylated product c.
[0071] Step 2) in the glass reactor equipped with thermometer, stirrer, dropping funnel and nitrogen inlet pipe, add 197g deionized water, add 25g acylate product c, 240g methyl butenyl polyethylene glycol ether ( Mn=2400g / mol), purging the reaction vessel with nitrogen while stirring, and heating up to 65°C to dissolve, then adding 1.65g of hydrogen peroxide (mass concentration: 30%), and stirring evenly. Then 0.41g of L-ascorbic acid, 64.5g of methacrylic acid, 1.65g of 3-mercaptopropionic acid, and 132g of water were mixed, stirred to form a uniform monomer aqueous solution, which was added dropwise to the reactor for 2 hours. After co...
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