A kind of preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retainer prepared by the method

A technology of slump-retaining agent and polycarboxylic acid, which is applied in the field of chemical building materials and construction, can solve the problems of double bond oxidation damage, polymerization activity influence, difficult-to-polymerize products, etc., so that it is not easy to self-polymerize, good for retention, and easy for esterification reaction Effect

Active Publication Date: 2016-03-09
KZJ NEW MATERIALS GROUP CO LTD
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Problems solved by technology

[0004] Chinese patent publication number CN101544729A discloses a kind of synthetic method of allyl polyethylene glycol acrylate, yet, because what this method uses is that acrylic acid and allyl polyethylene glycol carry out esterification, acrylic acid is higher than saturated acid anhydride when heated. It is easy to self-polymerize, therefore, it is necessary to add a polymerization inhibitor to prevent the polymerization of acrylic acid during the esterification process, and the added polymerization inhibitor will affect the polymerization during the copolymerization, so that more initiators need to be added during the 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. CN101851323A discloses a multi-branched polycarboxylate water reducer with excellent slump retention performance and its preparation method, but the monomer A used in its polymerization is: CH 3 O(CH 2 CH 2 O) n OCCH=CHCO(OCH 2 CH 2 ) n OCH 3 , where n is 6-20, the polymerization activity of this monomer will be seriously affected due to the long ether chain segments connected to both ends of the double bond, and it is difficult to polymerize to the final product during aqueous 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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  • A kind of preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retainer prepared by the method
  • A kind of preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retainer prepared by the method
  • A kind of preparation method of special slump retaining agent for cross-linked polycarboxylic acid and slump retainer prepared by the method

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Experimental program
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Effect test

Embodiment 1

[0044]Step 1, preparation of bifunctional 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. The temperature was raised to 60 °C, 1.06 g of concentrated sulfuric acid, and 1.00 g of p-toluenesulfonic acid were added, and the temperature was continued to slowly rise to 80 °C, kept at a constant temperature for 2 h, and cooled to 70 °C to obtain bifunctional macromonomers, unsaturated polyethers and unsaturated polyethers. Mixture A of saturated acid anhydride, total 182.41 g.

[0045] Step 2, copolymerization reaction: add 8.69 g of itaconic acid and 1.16 g of ammonium persulfate to the 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 add alkene dropwise. A mixed aqueous solution of sodium propyl sulfonate and isopropyl alcohol (including 11.08 g of sodium allyl sulfona...

Embodiment 2

[0048] Step 1, preparation of bifunctional macromonomer: 150.00g of 2-methylallyl polyethylene glycol (HPEG) with a molecular weight of 2400 and 27.04g of itaconic anhydride were added to the reactor, and under nitrogen protection, the temperature was increased. To 55°C, add 2.38g of concentrated sulfuric acid, continue to slowly heat up to 70°C, keep the temperature for 2 hours, and cool down to 60°C to obtain a mixture A containing bifunctional macromonomer, unsaturated polyether and unsaturated acid anhydride, with a total amount of 179.42g .

[0049] Step 2, copolymerization reaction: add 4.87 g of acrylic acid, 3.00 g of methacrylic acid, and 1.75 g of potassium persulfate to the reactor containing 179.42 g of mixture A, react at 60° C. for 1 h, then add 20.00 g of water, stir evenly, and then separate A mixed aqueous solution of sodium methacrylic acid sulfonate and mercaptopropionic acid (including 7.69 g of sodium methacrylic acid sulfonate, 0.72 g of mercaptopropionic...

Embodiment 3

[0052] Step 1, preparation of bifunctional macromonomer: 150.00 g of allyl polyethylene glycol (APEG) with a molecular weight of 1200 and 41.62 g of maleic anhydride were added to the reactor, and under nitrogen protection, the temperature was raised to 60 °C, 2.69 g of p-toluenesulfonic acid was added, the temperature was continued to slowly rise to 110 °C, the temperature was kept constant for 2.5 h, and the temperature was lowered to 70 °C to obtain a mixture A containing bifunctional macromonomer, unsaturated polyether and unsaturated acid anhydride, with a total amount of 194.31 g.

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

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Abstract

The invention discloses a method for preparing a special slump-retaining agent for cross-linked polycarboxylic acid. The steps are as follows: Step 1, preparation of a difunctional macromonomer: unsaturated polyether and unsaturated acid anhydride undergo partial esterification to form a bifunctional Mixture A of macromonomer, unsaturated polyether and unsaturated acid anhydride; Step 2, copolymerization reaction: carry out bulk polymerization with mixture A and unsaturated acid or unsaturated acid anhydride small monomer B under the effect of bulk polymerization initiator, and then Add sulfonic acid small monomer C and copolymerization modifier to carry out aqueous solution polymerization under the effect of aqueous solution initiator, obtain mass concentration and be the copolymerization product of 40%-80%; Step 3, neutralization reaction: adjust the pH value of copolymerization product 6-7, obtain special slump retaining agent for polycarboxylic acid. The invention also discloses a slump-retaining agent prepared by the preparation method of the special slump-retaining agent for cross-linked polycarboxylic acid. The invention achieves the effect of keeping the slump without loss through the introduction of the bifunctional macromonomer.

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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Patent Type & Authority Patents(China)
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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