CN115636614A - Polycarboxylate superplasticizer and preparation method thereof - Google Patents

Polycarboxylate superplasticizer and preparation method thereof Download PDF

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Publication number
CN115636614A
CN115636614A CN202211218978.6A CN202211218978A CN115636614A CN 115636614 A CN115636614 A CN 115636614A CN 202211218978 A CN202211218978 A CN 202211218978A CN 115636614 A CN115636614 A CN 115636614A
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China
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parts
raw materials
polycarboxylic acid
stirring
reducing agent
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CN202211218978.6A
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高艺玲
高浚峰
何小雄
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Hengyang Yinli Industrial Co ltd
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Hengyang Yinli Industrial Co ltd
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Abstract

The invention relates to a polycarboxylate superplasticizer and a preparation method thereof, wherein the polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 20-50 parts of polycarboxylic acid solution, 40-80 parts of acrylic polycarboxylic acid water reducing agent, 10-30 parts of early strength polycarboxylic acid water reducing agent, 30-50 parts of slump-retaining polycarboxylic acid water reducing agent, 25-45 parts of slow release polycarboxylic acid water reducing agent, 2-8 parts of polyether polyol A, 2-7 parts of polyether polyol B, 10-50 parts of halogenated fatty acid, 5-15 parts of hydroxypropyl methyl cellulose and 1-5 parts of hydrolyzed polymaleic anhydride. The polycarboxylate superplasticizer disclosed by the invention has good dispersibility, has very high fluidity in the application of high-strength concrete, and can greatly improve the strength of the formed concrete.

Description

Polycarboxylate superplasticizer and preparation method thereof
Technical Field
The invention relates to the technical field of production of polycarboxylic acid water reducing agents, and particularly relates to a polycarboxylic acid water reducing agent and a preparation method thereof.
Background
The polycarboxylate water reducing agent is a high-performance water reducing agent, and is a cement dispersing agent in the application of cement concrete. The mortar is widely applied to projects such as highways, bridges, dams, tunnels, high-rise buildings and the like, and along with the acceleration of the urbanization speed in China, various mortar products including self-leveling mortar, tile glue, grouting material and the like are increasingly widely used in civilian use and industry, so that higher requirements are provided for the performance of the mortar. The traditional mortar water reducer mainly comprises naphthalene and polyamines, and the conventional mortar water reducer greatly improves the fluidity, the workability, the strength and the like of mortar when applied to mortar products due to the high water reducing rate and the good fluidity retentivity of the conventional powder polycarboxylate water reducer, but the powder polycarboxylate water reducer forming technology is not mature and mainly shows the problems of high water content, low performance, flammability and the like of the powder polycarboxylate water reducer in the drying process for preparing the powder polycarboxylate water reducer.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a polycarboxylic acid water reducing agent and a preparation method thereof.
In order to achieve the above purpose, the invention provides the following technical scheme: the polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 20-50 parts of polycarboxylic acid solution, 40-80 parts of acrylic acid polycarboxylic acid water reducing agent, 10-30 parts of early strength polycarboxylic acid water reducing agent, 30-50 parts of slump retaining polycarboxylic acid water reducing agent, 25-45 parts of slow release polycarboxylic acid water reducing agent, 2-8 parts of polyether polyol A, 2-7 parts of polyether polyol B, 10-50 parts of halogenated fatty acid, 5-15 parts of hydroxypropyl methyl cellulose and 1-5 parts of hydrolyzed polymaleic anhydride.
Preferably, the raw materials of the polycarboxylate water reducer further comprise 5-12 parts of a compound agent, and the compound agent is a combination of polyethylene glycol diglycidyl ether, urotropine and ethanol.
More preferably, the polyether polyol A is a polypropylene oxide polyether polyol with a hydroxyl value of 200-300mgKOH/g, a functionality of 5-6 and a molecular weight of 300-500.
Further preferably, the raw materials of the polycarboxylate water reducer also comprise a protective colloid, and the protective colloid is prepared from polyvinyl alcohol, beta-cyclodextrin and methylated-beta-cyclodextrin according to the weight ratio of 1.3:1.7:2 to obtain a mixture.
The invention also comprises a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
the method comprises the following steps: preparing various raw materials, weighing the raw materials according to the proportioning weight of various components, putting the raw materials into a stirrer for stirring and mixing, sequentially putting the raw materials into the stirrer according to the putting sequence of the raw materials of the components in the mixing process, and simultaneously controlling the stirring temperature and the stirring time of the raw materials, wherein the stirring temperature is 40-50 ℃ and the stirring time is 1-2 hours;
step two: preparing a protective colloid, namely putting all raw materials for preparing the protective colloid into a stirrer to be stirred and mixed, and controlling the stirring temperature to be 30-40 ℃ and the stirring time to be 30-50min;
step three: putting the protective colloid obtained in the step two into the stirrer in the step one, and then stirring the protective colloid again at the stirring temperature of 30-40 ℃ for 10-20min to finally obtain the protective polycarboxylic acid water reducing agent;
step four: the finished product is detected, the finished product meeting the standard is filled in the containing barrel, and then the sealing treatment is carried out on the finished product.
In a further preferred mode, the outer surface of the finished product containing barrel in the fourth step is provided with a bar code, and the bar code is used for displaying the factory time, the shelf life aging and relevant information of the product.
In a further preferred mode, in the first step, the stirrer is used for stirring at a stirring speed of 1000r/min to obtain the primary polycarboxylic acid water reducing agent.
In a further preferred embodiment, the method for preparing the polycarboxylic acid water reducing agent further comprises the step of dropping a mixed solution of the unsaturated acid and the unsaturated amide monomer in the first step in the presence of a chain transfer agent to cause a radical copolymerization reaction.
In a further preferred aspect, the chain transfer agent is a thiol chain transfer agent.
In a further preferred embodiment, the first step is to add an initiator during stirring, the initiator being a free radical water soluble initiator, the initiator comprising an oxidizing component, or a combination of an oxidizing component initiator and a reducing component.
Compared with the prior art, the invention has the following beneficial effects:
the polycarboxylate water reducer disclosed by the invention has good dispersibility, has very high fluidity when being applied to high-strength-grade concrete, greatly improves the strength of formed concrete, has moderate air content, obviously improves the freeze-thaw resistance, is easy to pour and compact, greatly improves the components contained in the service life of the concrete, has high activity of epoxy groups at the end of a polyethylene glycol diglycidyl ether molecular chain, is easy to react with hydroxyl in hydroxypropyl methyl cellulose, and urotropine can promote the ring opening of the epoxy groups in the polyethylene glycol diglycidyl ether molecular chain and the cross-linking reaction with the hydroxypropyl methyl cellulose to form a three-dimensional network structure, and the network molecular chain formed by cross-linking has more hydrophilic groups and forms hydrogen bonds to attract water molecules. The polycarboxylate superplasticizer disclosed by the invention is green, environment-friendly and safe to use.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the polycarboxylate superplasticizer is prepared from the following raw materials in parts by weight: 20-50 parts of polycarboxylic acid solution, 40-80 parts of acrylic acid polycarboxylic acid water reducing agent, 10-30 parts of early strength polycarboxylic acid water reducing agent, 30-50 parts of slump retaining polycarboxylic acid water reducing agent, 25-45 parts of slow release polycarboxylic acid water reducing agent, 2-8 parts of polyether polyol A, 2-7 parts of polyether polyol B, 10-50 parts of halogenated fatty acid, 5-15 parts of hydroxypropyl methyl cellulose and 1-5 parts of hydrolyzed polymaleic anhydride.
In this embodiment, the raw materials of the polycarboxylate superplasticizer further include 5 to 12 parts of a compound agent, and the compound agent is a combination of polyethylene glycol diglycidyl ether, urotropine, and ethanol.
In this example, the polyether polyol A is a polypropylene oxide polyether polyol having a hydroxyl value of 200 to 300mgKOH/g, a functionality of 5 to 6, and a molecular weight of 300 to 500.
In this embodiment, the raw materials of the polycarboxylate water reducer further include a protective colloid, and the protective colloid is prepared from polyvinyl alcohol, β -cyclodextrin and methylated- β -cyclodextrin in a ratio of 1.3:1.7:2 to obtain a mixture.
Example 2:
the invention also comprises a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
the method comprises the following steps: preparing various raw materials, namely 20 parts of polycarboxylic acid solution, 40 parts of acrylic acid polycarboxylic acid water reducing agent, 10 parts of early strength polycarboxylic acid water reducing agent, 30 parts of slump retaining polycarboxylic acid water reducing agent, 25 parts of slow release polycarboxylic acid water reducing agent, 5 parts of polyether glycol A, 2 parts of polyether glycol B, 10 parts of halogenated fatty acid, 5-parts of hydroxypropyl methyl cellulose and 1 part of hydrolyzed polymaleic anhydride, weighing the raw materials according to the proportioning weight of the components, putting the raw materials into a stirrer to stir and mix, putting the raw materials into the stirrer in sequence according to the putting sequence of the raw materials of the components in the mixing process, and controlling the stirring temperature and the stirring time of the raw materials, wherein the stirring temperature is 40-50 ℃ and the stirring time is 1-2 hours;
step two: preparing a protective colloid, namely putting all raw materials for preparing the protective colloid into a stirrer to be stirred and mixed, and controlling the stirring temperature to be 30-40 ℃ and the stirring time to be 30-50min;
step three: putting the protective colloid obtained in the step two into the stirrer in the step one, and then stirring the protective colloid again at the stirring temperature of 30-40 ℃ for 10-20min to finally obtain the protective polycarboxylic acid water reducing agent;
step four: and detecting the finished product, filling the finished product meeting the standard into the containing barrel, and sealing the containing barrel.
Example 3:
the invention also comprises a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
the method comprises the following steps: preparing raw materials, namely 30 parts of a polycarboxylic acid solution, 45 parts of an acrylic acid polycarboxylic acid water reducing agent, 15 parts of an early strength polycarboxylic acid water reducing agent, 35 parts of a slump-retaining polycarboxylic acid water reducing agent, 25 parts of a slow release polycarboxylic acid water reducing agent, 2 parts of polyether polyol A, 2 parts of polyether polyol B, 10 parts of halogenated fatty acid, 5 parts of hydroxypropyl methyl cellulose and 1 part of hydrolyzed polymaleic anhydride, weighing the raw materials according to the proportioning weight of each component, putting the raw materials into a stirrer to be stirred and mixed, putting the raw materials into the stirrer according to the putting sequence of the raw materials of each component in the mixing process, and controlling the stirring temperature and the stirring time of the raw materials, wherein the stirring temperature is between 40 and 50 ℃, and the stirring time is between 1 and 2 hours;
step two: preparing a protective colloid, namely putting various raw materials for preparing the protective colloid into a stirrer for stirring and mixing, and controlling the stirring temperature to be 30-40 ℃ and the stirring time to be 30-50min;
step three: putting the protective colloid obtained in the step two into the stirrer in the step one, and then stirring the protective colloid again at the stirring temperature of 30-40 ℃ for 10-20min to finally obtain the protective polycarboxylate superplasticizer;
step four: the finished product is detected, the finished product meeting the standard is filled in the containing barrel, and then the sealing treatment is carried out on the finished product.
In this embodiment, the outer surface of the finished product containing barrel in the fourth step is provided with a bar code, and the bar code is used for displaying the delivery time, the shelf life aging and the relevant information of the product.
In this embodiment, in the first step, the stirrer stirs at a stirring speed of 1000r/min to obtain the primary polycarboxylic acid water reducing agent.
Example 4:
the invention also comprises a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
the method comprises the following steps: preparing raw materials, namely 50 parts of a polycarboxylic acid solution, 80 parts of an acrylic acid polycarboxylic acid water reducing agent, 30 parts of an early strength polycarboxylic acid water reducing agent, 50 parts of a slump-retaining polycarboxylic acid water reducing agent, 45 parts of a slow release polycarboxylic acid water reducing agent, 8 parts of polyether polyol A, 7 parts of polyether polyol B, 50 parts of halogenated fatty acid, 15 parts of hydroxypropyl methyl cellulose and 5 parts of hydrolyzed polymaleic anhydride, weighing the raw materials according to the proportioning weight of each component, putting the raw materials into a stirrer to be stirred and mixed, putting the raw materials into the stirrer according to the putting sequence of the raw materials of each component in the mixing process, and controlling the stirring temperature and the stirring time of the raw materials, wherein the stirring temperature is between 40 and 50 degrees, and the stirring time is between 1 and 2 hours;
step two: preparing a protective colloid, namely putting all raw materials for preparing the protective colloid into a stirrer to be stirred and mixed, and controlling the stirring temperature to be 30-40 ℃ and the stirring time to be 30-50min;
step three: putting the protective colloid obtained in the step two into the stirrer in the step one, and then stirring the protective colloid again at the stirring temperature of 30-40 ℃ for 10-20min to finally obtain the protective polycarboxylic acid water reducing agent;
step four: the finished product is detected, the finished product meeting the standard is filled in the containing barrel, and then the sealing treatment is carried out on the finished product.
In this embodiment, the preparation method of the polycarboxylic acid water reducing agent further includes, in the presence of a chain transfer agent, dropping a mixed solution of the unsaturated acid and the unsaturated amide monomer in the first step to generate a radical copolymerization reaction.
In this example, the chain transfer agent is a thiol chain transfer agent.
In this embodiment, the first step is to add an initiator while stirring, the initiator is a free radical water-soluble initiator, and the initiator comprises an oxidizing component or a combination of an oxidizing component initiator and a reducing component.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. The polycarboxylate superplasticizer is characterized by comprising the following raw materials in parts by weight: 20-50 parts of polycarboxylic acid solution, 40-80 parts of acrylic polycarboxylic acid water reducing agent, 10-30 parts of early strength polycarboxylic acid water reducing agent, 30-50 parts of slump-retaining polycarboxylic acid water reducing agent, 25-45 parts of slow release polycarboxylic acid water reducing agent, 2-8 parts of polyether polyol A, 2-7 parts of polyether polyol B, 10-50 parts of halogenated fatty acid, 5-15 parts of hydroxypropyl methyl cellulose and 1-5 parts of hydrolyzed polymaleic anhydride.
2. The polycarboxylate water reducer according to claim 1, characterized in that: the raw materials of the polycarboxylate superplasticizer also comprise 5-12 parts of a compound agent, and the compound agent is a combination of polyethylene glycol diglycidyl ether, urotropine and ethanol.
3. The polycarboxylate water reducer according to claim 1, characterized in that: the polyether polyol A is polypropylene oxide polyether polyol with a hydroxyl value of 200-300mgKOH/g, a functionality of 5-6 and a molecular weight of 300-500.
4. The polycarboxylate water reducer according to claim 1, characterized in that: the raw materials of the polycarboxylate superplasticizer further comprise a protective colloid, wherein the protective colloid is prepared from polyvinyl alcohol, beta-cyclodextrin and methylated-beta-cyclodextrin according to the weight ratio of 1.3:1.7:2 to obtain a mixture.
5. The invention also comprises a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
the method comprises the following steps: preparing various raw materials, weighing the raw materials according to the proportioning weight of various components, putting the raw materials into a stirrer for stirring and mixing, sequentially putting the raw materials into the stirrer according to the putting sequence of the raw materials of the components in the mixing process, and simultaneously controlling the stirring temperature and the stirring time of the raw materials, wherein the stirring temperature is 40-50 ℃ and the stirring time is 1-2 hours;
step two: preparing a protective colloid, namely putting all raw materials for preparing the protective colloid into a stirrer to be stirred and mixed, and controlling the stirring temperature to be 30-40 ℃ and the stirring time to be 30-50min;
step three: putting the protective colloid obtained in the step two into the stirrer in the step one, and then stirring the protective colloid again at the stirring temperature of 30-40 ℃ for 10-20min to finally obtain the protective polycarboxylic acid water reducing agent;
step four: the finished product is detected, the finished product meeting the standard is filled in the containing barrel, and then the sealing treatment is carried out on the finished product.
6. The preparation method of the polycarboxylate water reducer according to claim 5, characterized by comprising the following steps: and the outer surface of the finished product containing barrel in the fourth step is provided with a bar code, and the bar code is used for displaying factory time, shelf life aging and relevant information of products.
7. The method for preparing the polycarboxylate water reducer according to the claim 5, wherein the first step is to obtain the primary polycarboxylate water reducer by stirring with a stirrer at a stirring speed of 1000 r/min.
8. The preparation method of the polycarboxylate water reducer according to claim 5, characterized by comprising the following steps: the preparation method of the polycarboxylate superplasticizer further comprises the step of dropwise adding the mixed solution of the unsaturated acid and the unsaturated amide monomer in the first step in the presence of a chain transfer agent to carry out free radical copolymerization.
9. The preparation method of the polycarboxylate water reducer according to claim 8, characterized by comprising the following steps: the chain transfer agent is a mercaptan chain transfer agent.
10. The preparation method of the polycarboxylate water reducer according to claim 5, characterized by comprising the following steps: and step one, adding an initiator while stirring, wherein the initiator is a free radical water-soluble initiator and comprises an oxidation component or a composition of the oxidation component initiator and a reduction component.
CN202211218978.6A 2022-10-07 2022-10-07 Polycarboxylate superplasticizer and preparation method thereof Pending CN115636614A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116283030A (en) * 2023-05-18 2023-06-23 石家庄市长安育才建材有限公司 Early-strength viscosity-reducing water reducer and preparation method thereof

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CN107556442A (en) * 2017-09-30 2018-01-09 江苏兆佳建材科技有限公司 A kind of comprehensive polycarboxylate water-reducer of muting sensitive sense
EP3653592A1 (en) * 2018-11-16 2020-05-20 Shin-Etsu Chemical Co., Ltd. Water-reducing composition, hydraulic composition, and method for producing the same
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105130248A (en) * 2015-07-16 2015-12-09 岳阳东方雨虹防水技术有限责任公司 Composite polycarboxylic acid water reducing agent and preparation method thereof
CN105218760A (en) * 2015-11-09 2016-01-06 淄博德信联邦化学工业有限公司 The preparation method of polycarboxylate water-reducer
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116283030A (en) * 2023-05-18 2023-06-23 石家庄市长安育才建材有限公司 Early-strength viscosity-reducing water reducer and preparation method thereof
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Application publication date: 20230124