Method for preparing high-efficiency water-reducing agent of poly-carboxylic acid

A technology of high-efficiency water reducer and polycarboxylic acid, which is applied in the field of preparation of polycarboxylate high-efficiency water reducer, can solve the problems of difficult control of intermediate purity, cost increase, harsh reaction conditions, etc., and achieve the reduction of actual mixing water consumption, Improved strength and durability, and easy control of reaction conditions

Inactive Publication Date: 2008-12-31
SHENZHEN OCEANPOWER NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At home and abroad and in the literature, it is mentioned that the polymerization method for preparing polymers generally adopts a two-step method or a grafting method. The two-step method is more complicated to prepare the production process, and the reaction conditions are harsher and difficult to control, especially the preparation of the first step product. The obtained product contains too many impurities, which greatly affects the second-step polymerization reaction
Long production time, many restrictions, low efficiency, complex influencing factors, difficult to control the purity of intermediates, and some of the above preparation methods are carried out in organic solvents, which is not conducive to clean production and environmental protection
It also complicates the process, increases the cost, and brings inconvenience to production and use.
The polycarboxylate superplasticizer prepared by the two-step method has relatively large fluctuations in water reducing rate, poor adaptability to cement, poor compatibility with other admixtures, and poor temperature stability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 132g of water into the reaction kettle equipped with a thermometer, agitator, feeding port, reflux condenser, and nitrogen gas inlet pipe, pass in nitrogen gas to purge for 30min, heat in a water bath to 60°C, and then add 5.5g of methacrylic acid Sodium made the primer solution. The rotational speed of the stirrer was 60-100 rpm. Weigh 8.4g of acrylic acid and 30.9g of methoxypolyethylene glycol acrylate (n=9), and add 45g of water to form a mixed monomer solution. Weigh 3.6g of ammonium persulfate and add 68g of water to make an initiator. After the prepared mixed monomer solution and initiator were purged with nitrogen for 30 minutes, they were added dropwise to the reaction flask with a feeding pump respectively, and the dropping time was controlled at 3 hours. After the dropping, 27.2 g of initiator and The concentration is 14.2g of 30% methoxypolyethylene glycol acrylate (n=9) aqueous solution, the dropping time is controlled to 1h, and then the temperature ...

Embodiment 2

[0036] In a four-neck flask of a reaction kettle equipped with a thermometer, a stirrer, a dropping funnel, a reflux condenser, and a nitrogen inlet pipe, first replace the air in the bottle with nitrogen, and then add 6.5 g of sodium propylene sulfonate and 86 g of water to the bottle. A primer solution was formed and heated to 70°C in a water bath. The rotational speed of the stirrer was 60-100 rpm. Weigh 9.98g of methacrylic acid and 28.84g of methoxypolyoxyethylene methacrylate (n=23), add 45g of water to form a mixed monomer solution. Weigh 3.6g of ammonium persulfate and add 68g of water to make an initiator. After the configured mixed monomer solution and the initiator were purged with nitrogen for 30 minutes, they were added dropwise to the reaction flask with a feeding pump, and the dropping time was controlled at 4 hours. After the dropping, 27.2 g of the initiator and Concentration is 50% methoxy polyoxyethylene methacrylate (n = 23) aqueous solution 14.2g, dropwise...

Embodiment 3

[0040] In the four-necked flask of the reaction kettle equipped with a thermometer, agitator, dropping funnel, reflux condenser, and nitrogen gas introduction pipe, replace the air in the reaction kettle with nitrogen gas first, add 17g of water to the reaction kettle as the bottom material solution, and put it in a water bath Heat to 80°C. The rotational speed of the stirrer was 60-100 rpm. Weigh 35.67g methoxypolyethylene glycol methacrylate (n=35), 4.97g methacrylic acid and 2.4g mercaptoacetic acid, add 163g water to make a mixed monomer solution containing chain transfer agent, and then use carbonic acid Sodium hydrogen adjusts the pH of the mixed monomer solution to 5.0. Weigh 3.6g of ammonium persulfate and add 68g of water to make an initiator. After the configured mixed monomer solution and the initiator were purged with nitrogen for 30 minutes, they were added dropwise to the reaction flask with a feeding pump respectively, and the dropping time was controlled at 5...

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Abstract

The invention discloses a preparation method for a polycarboxylate high-performance water reducer, comprising the following steps: based on weight proportion, mixing 5-50% of unsaturated carboxylic acid, a derivative a of the unsaturated carboxylic acid, 45-95% of polyoxyethylene vinyl propionate ester, a derivative b of the polyoxyethylene vinyl propionate ester, as well as 0-30% of propyl sulfonate c to prepare a mixed monomer solution; then adding the initiator which takes up 0.5-15% of the total weight of the mixed monomer solution, and the chain transfer agent which takes up 0-15% of thetotal weight of the mixed monomer solution into the mixed monomer solution so as to prepare the polycarboxylate high-performance water reducer through binary or ternary copolymerization. The polycarboxylate high-performance water reducer disclosed in the invention can be widely applied to grout, mortar, concrete, gypsum and coal-water slurry, so that the mixed material can have higher mobility tosignificantly reduce the actual water consumption in the mixing process and effectively improve the concrete strength and durability, thereby showing the advantages of low mixing amount, high dispersion and high slump retaining performance.

Description

technical field [0001] The invention relates to a preparation method of a polycarboxylic acid high-efficiency water reducer. Background technique [0002] The early water reducing agents were mostly lignin sulfonate, naphthalene sulfonate formaldehyde condensate NSF, melamine sulfonate formaldehyde condensate MSF, aliphatic sulfamic acid ASPF, etc., which mainly played the role of reducing water, but There are problems such as high dosage, poor workability, poor adaptability, and large loss of concrete over time. If the dosage is too high, it will lead to poor water retention, severe segregation and bleeding, etc., making the concrete sticky, poor product stability, and difficult to modify. Simultaneous production and use all have pollution to the environment, use formaldehyde in its manufacturing process, can cause environmental pollution, slump loss through time is big and produce retardation; The naphthalene that uses is considered to be possible carcinogen, thereby has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B24/24C04B24/04C04B103/30
Inventor 刘方何唯平汤惠工罗英武
Owner SHENZHEN OCEANPOWER NEW MATERIALS TECH
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