Preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retaining agent prepared through method

A technology of slump-retaining agent and polycarboxylic acid, which is used in the field of chemical building materials and construction, can solve the problems of oxidative damage of double bonds, influence of polymerization activity, difficult polymerization products, etc., and achieves easy self-polymerization, favorable retention, and easy esterification reaction. Effect

Active Publication Date: 2014-06-04
KZJ NEW MATERIALS GROUP CO LTD
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  • Application Information

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Problems solved by technology

[0004] Chinese Patent Publication No. CN 101544729A discloses a kind of synthetic method of allyl polyethylene glycol acrylate, yet, because what this method uses is acrylic acid and allyl Polyethylene glycol is used for esterification, and acrylic acid is easier to self-polymerize than saturated acid anhydride when heated. Therefore, a polymerization inhibitor needs to be added during the esterification process to prevent the polymerization of acrylic acid, and the added polymerization inhibitor will affect polymerization during copolymerization, making Need to add more initiator during copolymerization
[0005] Moreover, in this method, because the selected acrylic acid will produce water during esterification, therefore, dry air is selected for carrying water, and it is considered that dry air can carry water , to increase the esterification rate, and the oxygen in the air can also inhibit the polymerization, but it is ignored that the double bonds of the unsaturated polyether itself and the double bonds in acrylic acid are easily oxidized by oxygen when the temperature is high destroy
[0006] Chinese Patent Publication No. CN 101851323A discloses a multi-branched polycarboxylate water reducer with excellent slump retention properties and its preparation method, but it is used when polymerizing The obtained monomer A is: CH3O(CH2CH2O)nOCCH=CHCO( OCH2CH2)nOCH3, where n is 6-20, the monomer is due to the double bond Both ends are connected with a longer ether chain segment, its polymerization activity will be seriously affected, and it is difficult to polymerize to the final product during aqueous solution polymerization
The monomer C used in it: CH2=C(R)CH2O(CH2CH2O)pM, where M is: -OCC(CH3)=CH or -OCCH=CH2 or -OCCH=CHCOOH , p is 15-120, R is H or CH3, this type of monomer also has the problem of low polymerization activity; and the polymerization activity of monomer A and monomer C is very low The copolymerization of monomers is more difficult

Method used

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  • Preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retaining agent prepared through method
  • Preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retaining agent prepared through method

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Experimental program
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Effect test

Embodiment 1

[0044]Step 1, preparation of difunctional macromonomers: 150.00 g of 3-methyl-3-butenyl polyethylene glycol (TPEG) with a molecular weight of 2400 and 30.35 g of maleic anhydride were added to the reactor, under nitrogen protection temperature to 60°C, add 1.06g of concentrated sulfuric acid and 1.00g of p-toluenesulfonic acid, continue to slowly raise the temperature to 80°C, keep the temperature for 2 hours, then cool down to 70°C to obtain difunctional macromonomer, unsaturated polyether and unsaturated polyether Mixture A of saturated anhydrides, total amount 182.41 g.

[0045] Step 2, copolymerization reaction: Add 8.69 g of itaconic acid and 1.16 g of ammonium persulfate to a reactor containing 182.41 g of mixture A, react at 70°C for 1.5 h, then add 60.00 g of water and stir evenly, and then dropwise add alkene Mixed aqueous solution of sodium propylsulfonate and isopropanol (ammonium persulfate 2.42g, water 30.00g) and ammonium persulfate aqueous solution (ammonium per...

Embodiment 2

[0048] Step 1, preparation of difunctional macromonomer: Add 150.00 g of 2-methallyl polyethylene glycol (HPEG) with a molecular weight of 2400 and 27.04 g of itaconic anhydride into the reactor, and raise the temperature under nitrogen protection To 55°C, add 2.38g of concentrated sulfuric acid, continue to raise the temperature slowly to 70°C, keep the temperature for 2h, and cool down to 60°C to obtain a mixture A containing difunctional macromonomer, unsaturated polyether and unsaturated acid anhydride, the total amount is 179.42g .

[0049] Step 2, copolymerization reaction: Add 4.87g of acrylic acid, 3.00g of methacrylic acid, and 1.75g ​​of potassium persulfate to a reactor containing 179.42g of mixture A, react at 60°C for 1h, then add 20.00g of water and stir evenly, and then separately A mixed aqueous solution of sodium methacrylsulfonate and mercaptopropionic acid (among them, 7.69 g of sodium methacrylsulfonate, 0.72 g of mercaptopropionic acid, and 30.00 g of wate...

Embodiment 3

[0052] Step 1, preparation of difunctional macromonomer: Add 150.00g of allyl polyethylene glycol (APEG) with a molecular weight of 1200 and 41.62g of maleic anhydride into the reactor, and raise the temperature to 60°C under the protection of nitrogen. Add 2.69g of p-toluenesulfonic acid, continue to slowly raise the temperature to 110°C, keep the temperature for 2.5h, and cool down to 70°C to obtain a mixture A containing difunctional macromonomer, unsaturated polyether and unsaturated acid anhydride, with a total amount of 194.31g.

[0053] Step 2, copolymerization reaction: Add 12.66g of methacrylic acid and 1.31g of ammonium persulfate to a reactor containing 194.31g of mixture A, react at 50°C for 0.5h, then add 1.00g of potassium persulfate, and react at 70°C 0.5h, then add 70.00g of water and stir evenly, then add dropwise the mixed aqueous solution of sodium styrene sulfonate and thioglycolic acid (among them, 9.50g of sodium styrene sulfonate, 1.08g of thioglycolic ac...

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Abstract

The invention discloses a preparation method of a special slump retaining agent for cross-linked polycarboxylic acid. The preparation method comprises the following steps of step I, preparing a difunctional macromonomer: partially esterifying unsaturated polyether and unsaturated anhydride to generate a mixture A of the difunctional macromonomer, the unsaturated polyether and the unsaturated anhydride; step II, copolymerizing: polymerizing the mixture and unsaturated acid or unsaturated hydride small monomer B in the presence of a body polymerization initiator, adding sulfonic acid small monomer C and copolymerization adjusting agent to have the aqueous solution polymerization in the presence of an aqueous solution initiator to obtain a copolymerization product with mass concentration of 40 to 80 percent; step III, neutralizing: adjusting the pH value of the copolymerization product to be 6 to 7 to obtain special slump retaining agent for polycarboxylic acid. The invention also discloses a slump retaining agent prepared through the preparation method of the slump retaining agent for the cross-linked polycarboxylic acid. By introducing the difunctional macromonomer, an effect for preventing the slump loss can be realized.

Description

technical field [0001] The invention belongs to the technical field of chemical building materials construction, and in particular relates to a method for preparing a special slump-retaining agent for cross-linked polycarboxylic acid and the slump-retaining agent prepared by the method. Background technique [0002] The excellent water-reducing performance of polycarboxylate superplasticizers has been widely recognized by the industry, but due to factors such as changes in cement, mud content in sand, and stone materials, polycarboxylate superplasticizers have also slumped in practical applications. The problem of excessive loss of speed. [0003] Therefore, it is very necessary and urgent to develop a special slump-retaining agent for polycarboxylic acid. This type of slump-retaining agent needs to have good compatibility with the existing polycarboxylate superplasticizer, and needs to be compatible with cement, sand, stone, etc. The material has good adaptability and can ...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F220/06C08F222/02C08F222/06C08F222/04C08F228/02C08F212/14C08F220/58C08F2/02C08F2/10C04B24/16C04B103/30
Inventor 蒋卓君郭鑫祺方云辉官梦芹李英祥
Owner KZJ NEW MATERIALS GROUP CO LTD
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