6C polyether macromonomer high-water-reduction powder water reducer

Abstract

The invention discloses a 6C polyether macromonomer high-water-reduction powder water reducer and a preparation method thereof. The 6C polyether macromonomer high-water-reduction powder water reducer comprises a polyether macromonomer, water, organic acid, an oxidizing agent, a reducing agent and a chain transfer agent. According to the 6C polyether macromonomer high-water-reduction powder water reducer and the preparation method thereof, the powder water reducer can be obtained by optimizing components and adjusting a molecular structure, the water reduction performance of the water reducer is effectively improved, continuous production in a low-temperature / normal-temperature environment can be realized, the production efficiency is greatly improved, the safety risk is reduced, and the product quality is improved. And the purposes of energy conservation and emission reduction are achieved.

Description

Technical Field

[0001] The invention relates to the technical field of cement / gypsum-based mortar, and in particular to a 6C polyether macromonomer high water-reducing powder water-reducing agent. Background Art

[0002] At present, with the introduction of 6C polyether macromonomer, a large number of scholars or technicians have studied its application in water reducers. For example, Chinese patent CN112480330A discloses the application of a new EPEG polyether macromonomer in low-temperature synthesis of viscosity-reducing water reducer. The water reducer has viscosity reduction performance, as well as water reduction, slump retention and mud resistance performance; CN111620986A discloses a method for synthesizing a low-sensitivity polycarboxylic acid mother liquor, in which EPEG3000 is used to synthesize a polymer with a low acid-ether ratio at low temperature, and the polycarboxylic acid mother liquor prepared by introducing acrylic ester has the characteristics of moderate water reduction rate and slump retention, which solves the problem of high sensitivity of commonly used carboxylic acid mother liquor.

[0003] However, the prior art has at least the following disadvantages: 1. The existing technology has little research on the powdering properties of 6C polyether macromonomers, and most of them are focused on the development of liquid water reducers, which limits the application of this type of monomer in dry mortar systems; 2. Currently, the research focuses on monomers with a molecular weight of 3000. There is less research on the performance of monomers with higher molecular weights of 4000, 5000, and even 6000. The performance advantages of 6C polyether macromonomers are not fully utilized, and the performance of water reducers needs to be improved. Summary of the invention

[0004] In order to solve the above technical problems, a technical solution adopted by the present invention is: Provided is a 6C polyether macromonomer high water-reducing powder water reducer, the components and the content of each component of the 6C polyether macromonomer include: in parts by weight, 42-45 parts of polyether macromonomer, 50-55 parts of water, 4-6 parts of organic acid, 0.5-0.7 parts of oxidant, 0.08-0.1 parts of reducing agent, 0.5-1 parts of chain transfer agent and 0.3-0.8 parts of antioxidant, wherein the polyether macromonomer is ethylene glycol monovinyl polyethylene glycol ether, and the molecular weight of the polyether macromonomer is greater than or equal to 4000.

[0005] In a preferred embodiment of the present invention, the molecular weight of the polyether macromonomer includes 4000, 5000, and 6000.

[0006] In a preferred embodiment of the present invention, the organic acid includes one or more of acrylic acid, methacrylic acid, maleic anhydride, itaconic acid, and 2-acrylamide-2-methylpropanesulfonic acid.

[0007] In a preferred embodiment of the present invention, the oxidant includes one or two of hydrogen peroxide, ammonium persulfate, potassium persulfate, and tert-butyl hydroperoxide.

[0008] In a preferred embodiment of the present invention, the reducing agent includes one or more of E51, L-ascorbic acid, sodium bisulfite formaldehyde, sodium sulfite, sodium thiosulfate, sodium hypophosphite, sodium phosphite and ferrous chloride.

[0009] In a preferred embodiment of the present invention, the chain transfer agent includes one or more of mercaptoethanol, thioglycolic acid, mercaptopropionic acid, sodium hypophosphite, hypophosphorous acid, sodium propylene sulfonate, and sodium methpropylene sulfonate.

[0010] In a preferred embodiment of the present invention, the preparation method comprises: Step 1: Add 42-45 parts of polyether macromonomer and 40-45 parts of deionized water into a reaction kettle, stir and dissolve them at room temperature to obtain a base liquid for standby use; Step 2: Prepare dropwise addition material a by mixing 4-6 parts of organic acid, 0.5-1 parts of chain transfer agent and 4-6 parts of water; prepare dropwise addition material b by mixing 0.08-0.1 parts of reducing agent and 6-8 parts of water; Step 3: Add 0.5-0.7 parts of oxidant to the base material, then drop material a and material b into the mixed solution, heat to 10-40°C for reaction for 1-3h, keep warm for 1h after the reaction, then adjust the pH to 6-7 to obtain a water reducing agent mother solution; Step 4: Add 0.3-0.8 parts of antioxidant to the water reducing agent mother liquor and perform centrifugal drying and spraying to obtain a powdered water reducing agent.

[0011] In a preferred embodiment of the present invention, 32 parts by weight of sodium hydroxide are added in the third step for neutralization.

[0012] In a preferred embodiment of the present invention, the concentration of the water reducing agent mother solution prepared in the third step is 50%.

[0013] The beneficial effects of the present invention are: a powder water reducer can be obtained by optimizing components and adjusting molecular structure, and the water reducing performance of the water reducer is effectively improved, and continuous production under low temperature / normal temperature environment can be achieved, which greatly improves production efficiency, reduces safety risks, and achieves the purpose of energy saving and emission reduction. DETAILED DESCRIPTION

[0014] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0015] The embodiments of the present invention include: A 6C polyether macromonomer high water-reducing powder water reducer is a high water-reducing powder water reducer suitable for various mortar systems, especially gypsum-based self-leveling and cement-based self-leveling. Its components and the content of each component include: in parts by weight, 42-45 parts of polyether macromonomer, 50-55 parts of water, 4-6 parts of organic acid, 0.5-0.7 parts of oxidant, 0.08-0.1 parts of reducing agent, and 0.5-1 parts of chain transfer agent. The polyether macromonomer includes EPEG and 6C polyether macromonomer, and the molecular weight of the polyether macromonomer includes 4000, 5000, and 6000.

[0016] More preferably, the organic acid includes one or more of acrylic acid, methacrylic acid, maleic anhydride, itaconic acid, and 2-acrylamide-2-methylpropanesulfonic acid.

[0017] More preferably, the oxidant includes one or two of hydrogen peroxide, ammonium persulfate, potassium persulfate, and tert-butyl hydroperoxide.

[0018] Further preferably, the reducing agent includes one or more of E51 (sodium dioctyl sulfosuccinate), L-ascorbic acid, sodium bisulfite formaldehyde, sodium sulfite, sodium thiosulfate, sodium hypophosphite, sodium phosphite and ferrous chloride.

[0019] Further preferably, the chain transfer agent includes one or more of mercaptoethanol, thioglycolic acid, mercaptopropionic acid, sodium hypophosphite, hypophosphorous acid, sodium propylene sulfonate, and sodium methpropylene sulfonate. Specific embodiments

[0020] The preparation method of the water reducing agent comprises: (1) Fully dissolve 360 ​​g of EPEG 4000 molecular weight, 300 g of water and 8 g of sodium hypophosphite to prepare a base material; (2) Preparation of dropwise addition material a: 49 g acrylic acid and 50 g water; (3) Prepare dropwise addition material b: VC 0.8 g, water 58 g; (4) Add 3.85 g of hydrogen peroxide and 0.02 g of ferrous sulfate to the base material, add material a dropwise for 1 hour, add material b dropwise for 1.5 hours, raise the temperature to 15-35°C for reaction, keep the temperature for 1 hour after the reaction is completed, and then add alkali for neutralization to obtain water reducer mother solution A; Specific embodiments

[0021] The preparation method of the water reducing agent comprises: (1) Fully dissolve 360 ​​g of EPEG 5000 molecular weight, 300 g of water, and 8 g of sodium methyl methacrylate sulfonate to prepare a base material; (2) Prepare dropwise addition material a: 44 g acrylic acid, 2 g R material - mercaptopropionic acid, 50 g water; (3) Prepare dropwise addition material b: 0.6 g E51 and 58 g water; (4) Add 4.2 g of hydrogen peroxide and 0.06 g of ferrous sulfate to the base material, add a and b dropwise for 40 min and 50 min respectively, raise the temperature to 10-35 °C for reaction, keep the temperature for 1 h after the reaction is completed, add alkali for neutralization, and obtain water reducer mother solution B. Specific embodiments

[0022] The preparation method of the water reducing agent comprises: (1) Fully dissolve 360 ​​g of EPEG 6000 molecular weight and 300 g of water to prepare a base material; (2) Preparation of dropwise addition material a: 38 g acrylic acid, 40 g water, and 2 g mercaptoethanol; (3) Prepare dropwise addition material b: 0.65 g E51 and 58 g water; (4) Add 4.25 g of hydrogen peroxide and 0.09 g of ferrous sulfate to the base material, add a and b dropwise for 35 min and 50 min respectively, raise the temperature to 10-35 °C for reaction, keep the temperature for 1 h after the reaction is completed, add alkali for neutralization, and obtain water reducer mother solution C.

[0023] Self-leveling test: Water-reducing agent mother liquor A, water-reducing agent mother liquor B and water-reducing agent mother liquor C were neutralized to about pH 8, antioxidants were added and centrifugal drying spray was performed to obtain powder water-reducing agent A, powder water-reducing agent B and powder water-reducing agent C with good fluidity; powder water-reducing agent A, powder water-reducing agent B and powder water-reducing agent C were subjected to gypsum-based / cement-based self-leveling tests respectively.

[0024] As shown in the table below, after testing, the performance of the three groups of powders is better than the commercially available powders PC1 and PC2, and all reach a relatively high level in the market.

[0025] (1) Desulfurized gypsum-based self-leveling

[0026] (2) Phosphogypsum-based self-leveling

[0027] (3) Cement-based self-leveling

[0028] The beneficial effects of the 6C polyether macromonomer high water-reducing powder water-reducing agent and the preparation method thereof of the present invention are: 1. By using higher molecular weight monomers such as EPEG to achieve low temperature / normal temperature reaction process, the water reducing performance of water reducer can be effectively improved; 2. Use a variety of redox systems to achieve room for optimizing polymer performance under different conditions; 3. Explore the correlation between different molecular structures and powder formation, optimize the structure, use a composite chain transfer agent, adjust the molecular structure, and achieve diversification of molecular weight distribution structure, so that 6C polyether macromonomer can be dried and sprayed into powder; 4. Adding antioxidants during the drying and spraying process can solve the risk of flammable powders in the drying and spraying process, and can achieve continuous production for at least one week in the factory, which can not only greatly improve production capacity and efficiency, but also achieve the goal of energy conservation and emission reduction.

[0029] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A 6C polyether macromonomer high water reducing powder water reducing agent, characterized in that: The components and the contents of each component include: in parts by weight, 42-45 parts of polyether macromonomer, 50-55 parts of water, 4-6 parts of organic acid, 0.5-0.7 parts of oxidant, 0.08-0.1 parts of reducing agent, 0.5-1 parts of chain transfer agent and 0.3-0.8 parts of antioxidant, wherein the polyether macromonomer is ethylene glycol monovinyl polyethylene glycol ether, and the molecular weight of the polyether macromonomer is greater than or equal to 4000.

2. A 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: The molecular weight of the polyether macromonomer includes 4000, 5000, and 6000.

3. A 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: The organic acid includes one or more of acrylic acid, methacrylic acid, maleic anhydride, itaconic acid, and 2-acrylamide-2-methylpropanesulfonic acid.

4. A 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: The oxidant includes one or two of hydrogen peroxide, ammonium persulfate, potassium persulfate, and tert-butyl hydroperoxide.

5. A 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: The reducing agent includes one or more of E51, L-ascorbic acid, sodium bisulfite formaldehyde, sodium sulfite, sodium thiosulfate, sodium hypophosphite, sodium phosphite and ferrous chloride.

6. A 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: The chain transfer agent includes one or more of mercaptoethanol, thioglycolic acid, mercaptopropionic acid, sodium hypophosphite, hypophosphorous acid, sodium propylene sulfonate, and sodium methpropylene sulfonate.

7. The 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: The preparation method thereof comprises: Step 1: Add 42-45 parts of polyether macromonomer and 40-45 parts of deionized water into a reaction kettle, stir and dissolve them at room temperature to obtain a base liquid for standby use; Step 2: Prepare dropwise addition material a by mixing 4-6 parts of organic acid, 0.5-1 parts of chain transfer agent and 4-6 parts of water; prepare dropwise addition material b by mixing 0.08-0.1 parts of reducing agent and 6-8 parts of water; Step 3: Add 0.5-0.7 parts of oxidant to the base material, then drop material a and material b into the mixed solution, heat to 10-40°C for reaction for 1-3h, keep warm for 1h after the reaction, then adjust the pH to 6-7 to obtain a water reducing agent mother solution; Step 4: Add 0.3-0.8 parts of antioxidant to the water reducing agent mother liquor and perform centrifugal drying and spraying to obtain a powdered water reducing agent.

8. The 6C polyether macromonomer high water reducing powder water reducer according to claim 1, characterized in that: In the third step, 32 parts by weight of sodium hydroxide are added for neutralization.

9. The 6C polyether macromonomer high water reducing powder water reducing agent according to claim 1, characterized in that: The concentration of the water reducing agent mother solution prepared in the third step is 50%.

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