CN113087433B - Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof - Google Patents
Viscosity-reducing polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
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Abstract
The application relates to the field of water reducing agents, and discloses a viscosity reduction type polycarboxylate water reducing agent and a preparation method thereof. The viscosity reduction type polycarboxylate superplasticizer comprises the following raw materials in parts by weight: 5-8 parts of methacrylic acid; 15-20 parts of acrylic acid; 2-3 parts of methoxy polyethylene glycol acrylate; 1-2 parts of sodium methallyl sulfonate; 1-2 parts of an initiator; 4-5 parts of 3-oxetanone; 1.5-2 parts of dimethyl sebacate; 40-50 parts of water; the preparation method comprises the following steps: mixing 3-oxetanone and dimethyl sebacate, and adding the mixture into a polycarboxylic acid product mixed with water to obtain a water reducing agent; the application has the following advantages and effects: the mixed product of 3-oxetanone and dimethyl sebacate is further added into the conventional polycarboxylic acid water reducing agent component, so that the mixed product is diffused among cement particles, is combined with oily molecules through heterocyclic atoms, reduces the generation of complex among the cement particles by the special spatial configuration of the 3-oxetanone, reduces the aggregation among the cement particles, realizes the purpose of reducing viscosity and reduces the viscosity of concrete.
Description
Technical Field
The application relates to the field of water reducing agents, in particular to a viscosity reduction type polycarboxylate water reducing agent and a preparation method thereof.
Background
When concrete with higher strength grade is prepared, a high-performance water reducing agent with high water reducing rate is usually selected. The polycarboxylic acid water reducing agent has the excellent performances of high water reducing rate, obvious reinforcing effect, low slump loss of concrete mixtures and the like, and becomes a hotspot for research and development of water reducing agents at home and abroad.
At present, a patent with publication number CN106348635A discloses a polycarboxylic acid water reducing agent, which is composed of the following raw materials in parts by weight: 10-15 parts of isobutylene alcohol polyoxyethylene ether, 5-8 parts of tartaric acid, 1-3 parts of acrylic acid, 0.5-2 parts of sodium methallyl sulfonate, 1-2 parts of p-hydroxybenzoate preservative and 10-20 parts of water.
Nowadays, some high-strength or ultra-high-strength concrete has high viscosity and low flowing speed due to the characteristics of high glue material and low water-glue ratio, and the polycarboxylic acid water reducing agent still cannot meet the performance requirement of reducing the viscosity of the concrete, so the improvement is still needed.
Disclosure of Invention
In order to reduce the viscosity of concrete and improve the flowing speed, the application provides a viscosity-reducing polycarboxylic acid water reducer and a preparation method thereof.
In a first aspect, the application provides a viscosity reduction type polycarboxylate superplasticizer, which adopts the following technical scheme:
the viscosity-reducing polycarboxylate superplasticizer comprises the following raw materials in parts by weight:
5-8 parts of methacrylic acid;
15-20 parts of acrylic acid;
2-3 parts of methoxy polyethylene glycol acrylate;
1-2 parts of sodium methallyl sulfonate;
1-2 parts of an initiator;
4-5 parts of 3-oxetanone;
1.5-2 parts of dimethyl sebacate;
40-50 parts of water.
By adopting the technical scheme, methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate generate the polycarboxylic acid water reducer under the action of an initiator; the 3-oxetanone and dimethyl sebacate are further added, the product obtained by mixing the 3-oxetanone and the dimethyl sebacate can diffuse among cement particles along with the addition of a water reducing agent, and is combined with oily molecules through heterocyclic atoms, and the generation of a complex among the cement particles is reduced by the special spatial configuration of the 3-oxetanone, so that aggregates of the cement particles are separated and transformed into irregular distribution, the molecular structure becomes loose, the order degree is reduced, the entropy is increased, the aggregation among the cement particles is reduced, and the intermolecular force is also reduced, so that a better viscosity reducing effect is obtained, the viscosity of concrete is reduced, and the pumping efficiency and the construction progress are improved.
Preferably: the raw material also comprises 2-3 parts of 2-pyridine boric acid by weight.
By adopting the technical scheme, when the 2-pyridine boric acid is mixed in the concrete, the 2-pyridine boric acid has higher charge density and stronger coordination effect on calcium ions, so that the cement particles can be better coated, the internal friction among the cement particles in the concrete is reduced, and the aim of effectively reducing the viscosity of the concrete is fulfilled.
Preferably: the raw material also comprises 3-4 parts of glyceryl oleate according to parts by weight.
By adopting the technical scheme, the polar glyceryl oleate is further added to be mixed with the 2-pyridine boric acid, the increase of the polarity can improve the surface tension, so that the 2-pyridine boric acid has stronger adsorption capacity on cement particles, the cement particles are better dispersed, and a stable adsorption layer is formed on the surfaces of the cement particles, thereby effectively reducing the internal friction among the cement particles, producing better viscosity reducing effect and reducing the viscosity of concrete.
Preferably: the raw materials also comprise 1-2 parts of octadecylamine according to parts by weight.
By adopting the technical scheme, the addition of the long straight-chain alkane octadecylamine has good space extension effect and shielding effect, can prevent the accumulation of cement particles and also can loosen the accumulation structure; meanwhile, the octadecylamine has good interfacial activity and larger molecular diffusion, and can reduce the cohesion of concrete, thereby reducing the internal friction force of the concrete during flowing and reducing the viscosity of the concrete; in addition, the octadecyl amine accounts for 1-2 parts, so that the dosage is reduced, and the influence of long-chain alkyl amine with lower polarity on the polarity effect of the glyceryl oleate is avoided.
Preferably: the raw materials also comprise 0.5 to 0.6 portion of laureth by weight.
By adopting the technical scheme, the laureth is added and mixed with the octadecylamine, so that the interfacial compatibility of the octadecylamine and the rest of the components of the water reducing agent is improved, and the performance of the water reducing agent is better improved.
Preferably: the initiator is ammonium persulfate.
In a second aspect, the application provides a preparation method of a viscosity-reducing polycarboxylate superplasticizer, which adopts the following technical scheme: a preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40-45 ℃, and stirring for 30-40min to obtain a heterocyclic product; under the condition of a thermostatic water bath at 90-95 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3-4h, continuously preserving heat for 1h, and adjusting the pH value to 5-6 by using a 30% NaOH solution; then cooling to 50-60 ℃, adding the prepared heterocyclic ring product, and stirring for 18-20min to obtain the water reducing agent.
Preferably: fully mixing 2-3 parts of 2-pyridine boric acid and 0.6-0.8 part of glyceryl oleate, heating to 30-40 ℃, and stirring for 15-25min to obtain a coordination mixture;
mixing 2-3 parts of octadecylamine and 0.5-0.6 part of laureth to obtain a straight-chain mixture;
adjusting pH to 5-6 with 30% NaOH solution, cooling to 50-60 deg.C, adding heterocyclic mixture obtained by stirring 4-5 parts of 3-oxetanone and 1.5-2 parts of dimethyl sebacate at 40-45 deg.C for 30-40min, and continuing stirring for 18-20 min; then adding the coordination mixture, and stirring for 20-25 min; and adding the straight chain mixture, and continuously stirring for 30-40min to obtain the water reducing agent.
In summary, the present application has the following beneficial effects:
1. the polycarboxylic acid water reducer is generated by adopting methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate under the action of an initiator; further adding a mixed product of 3-oxetanone and dimethyl sebacate, enabling the mixed product to diffuse among cement particles, combining heterocyclic atoms with oily molecules, reducing the generation of complex among the cement particles by using the special spatial configuration of the 3-oxetanone, reducing the aggregation among the cement particles, obtaining a better viscosity reducing effect and reducing the viscosity of concrete;
2. in the application, 2-pyridine boric acid with higher charge density and stronger coordination effect on calcium ions is preferably adopted, and polar glyceryl oleate is added for mixing, so that the cement particles can be better coated to form a stable adsorption layer, the internal friction among the cement particles in the concrete is reduced, and the purpose of effectively reducing the viscosity of the concrete is achieved;
3. according to the concrete water reducing agent, long straight-chain alkane octadecylamine is added, interfacial compatibility of the octadecylamine and the rest of components of the water reducing agent is improved through lauryl polyether, a good space extension effect and a good shielding effect are achieved, accumulation and aggregation of cement particles are hindered, the molecular diffusion degree is improved, and the internal friction force of concrete during flowing is reduced.
Detailed Description
The present application will be described in further detail with reference to examples.
In the application, the methoxy polyethylene glycol acrylate is purchased from Liyang Ruipu New Material Co., Ltd, and the model is MPEG 400A; 3-Oxetanone is available from Gilat chemical Co., Ltd, Jiaxing; dimethyl sebacate was purchased from Hangzhou Suiyang science and technology, Inc.; the glyceryl oleate is purchased from Jiaxing Zhongcheng environmental protection science and technology GmbH, and has a molecular weight of 356; 2-pyridine boric acid is purchased from chemical engineering Limited company Wangdai Hubei, and has the purity of 99 percent; octadecylamine was purchased from denayan chemical ltd; the laureth is laureth-4 which is chemically synthesized; the water in the examples of the present application is deionized water.
The raw materials used in the following embodiments may be those conventionally commercially available unless otherwise specified.
Examples
Example 1
The application discloses a viscosity-reducing polycarboxylate water reducer, which comprises raw materials of methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate, an initiator, 3-oxetanone, dimethyl sebacate and water, wherein the initiator is ammonium persulfate, and the content of each component is shown in the following table 1.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40 ℃, and stirring for 30min to obtain a heterocyclic product;
under the condition of a constant-temperature water bath at 90 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 5 by using a 30% NaOH solution; then cooling to 50 ℃, adding the prepared heterocyclic ring product, and stirring for 18min to obtain the water reducing agent.
Example 2
The application discloses a viscosity-reducing polycarboxylate water reducer, which comprises raw materials of methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate, an initiator, 3-oxetanone, dimethyl sebacate and water, wherein the initiator is potassium persulfate, and the content of each component is shown in the following table 1.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 45 ℃, and stirring for 40min to obtain a heterocyclic product;
under the condition of a constant-temperature water bath at 95 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 4 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 6 by using a 30% NaOH solution; then cooling to 60 ℃, adding the prepared heterocyclic ring product, and stirring for 20min to obtain the water reducing agent.
Example 3
The application discloses a viscosity-reducing polycarboxylate water reducer, which comprises raw materials of methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate, an initiator, 3-oxetanone, dimethyl sebacate and water, wherein the initiator is ammonium persulfate, and the content of each component is shown in the following table 1.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 43 ℃, and stirring for 35min to obtain a heterocyclic product;
under the condition of a constant-temperature water bath at 92 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 6 by using a 30% NaOH solution; then cooling to 55 ℃, adding the prepared heterocyclic ring product, and stirring for 19min to obtain the water reducing agent.
Example 4
The application discloses a viscosity-reducing polycarboxylic acid water reducer, which comprises raw materials of methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate, an initiator, 3-oxetanone, dimethyl sebacate, water, 2-pyridine boric acid, glycerol oleate, octadecyl amine and laureth, wherein the initiator is ammonium persulfate, and the content of each component is shown in the following table 1.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40 ℃, and stirring for 30min to obtain a heterocyclic product;
fully mixing 2-pyridine boric acid and glyceryl oleate, heating to 30 ℃, and stirring for 15min to obtain a coordination mixture;
mixing octadecyl amine and laurinol polyether to obtain a straight chain mixture;
under the condition of a constant-temperature water bath at 90 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3, continuously preserving heat for 1h, and adjusting the pH value to 5 by using a 30% NaOH solution; then cooling to 50 ℃, adding the prepared heterocyclic product, and stirring for 18 min; then adding the coordination mixture, and stirring for 20 min; and adding the straight chain mixture, and continuously stirring for 30min to obtain the water reducing agent.
Example 5
The application discloses a viscosity-reducing polycarboxylic acid water reducer, which comprises raw materials of methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate, an initiator, 3-oxetanone, dimethyl sebacate, water, 2-pyridine boric acid, glycerol oleate, octadecyl amine and laureth, wherein the initiator is ammonium persulfate, and the content of each component is shown in the following table 1.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 45 ℃, and stirring for 40min to obtain a heterocyclic product;
fully mixing 2-pyridine boric acid and glyceryl oleate, heating to 40 ℃, and stirring for 25min to obtain a coordination mixture;
mixing octadecyl amine and laurinol polyether to obtain a straight chain mixture;
under the condition of a constant-temperature water bath at 95 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 4 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 6 by using a 30% NaOH solution; then cooling to 60 ℃, adding the prepared heterocyclic product, and stirring for 20 min; then adding the coordination mixture, and stirring for 25 min; and adding the straight chain mixture, and continuously stirring for 40min to obtain the water reducing agent.
Example 6
The application discloses a viscosity-reducing polycarboxylic acid water reducer, which comprises raw materials of methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate, an initiator, 3-oxetanone, dimethyl sebacate, water, 2-pyridine boric acid, glycerol oleate, octadecyl amine and laureth, wherein the initiator is ammonium persulfate, and the content of each component is shown in the following table 1.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 43 ℃, and stirring for 5min to obtain a heterocyclic product;
fully mixing 2-pyridine boric acid and glyceryl oleate, heating to 35 ℃, and stirring for 20min to obtain a coordination mixture;
mixing octadecyl amine and laurinol polyether to obtain a straight chain mixture;
under the condition of a constant-temperature water bath at 92 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 6 by using a 30% NaOH solution; then cooling to 55 ℃, adding the prepared heterocyclic product, and stirring for 19 min; then adding the coordination mixture, and stirring for 23 min; and adding the straight chain mixture, and continuously stirring for 35min to obtain the water reducing agent.
Example 7
The difference from the example 1 is that the raw material of the viscosity-reducing type polycarboxylate superplasticizer further comprises 2-pyridine boric acid, and the content of each component is shown in the following table 2.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40 ℃, and stirring for 30min to obtain a heterocyclic product;
under the condition of a constant-temperature water bath at 90 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 5 by using a 30% NaOH solution; then cooling to 50 ℃, adding the prepared heterocyclic product, and stirring for 18 min; then adding 2-pyridine boric acid, and stirring for 20min to obtain the water reducing agent.
Example 8
The difference from example 7 is that the raw material of the viscosity-reducing type polycarboxylate superplasticizer further comprises glyceryl oleate, and the content of each component is shown in the following table 2.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40 ℃, and stirring for 30min to obtain a heterocyclic product;
fully mixing 2-pyridine boric acid and glyceryl oleate, heating to 30 ℃, and stirring for 15min to obtain a coordination mixture;
under the condition of a constant-temperature water bath at 90 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 5 by using a 30% NaOH solution; then cooling to 50 ℃, adding the prepared heterocyclic product, and stirring for 18 min; and then adding the coordination mixture, and stirring for 20min to obtain the water reducing agent.
Example 9
The difference from example 1 is that the raw material of the viscosity-reducing type polycarboxylate superplasticizer further comprises glyceryl oleate, and the content of each component is shown in the following table 2.
Example 10
The difference from example 7 is that 2-pyridineboronic acid was replaced with acetic acid and the contents of the components are shown in table 2 below.
Example 11
The difference from example 8 is that glycerol oleate is replaced by glycerol allyl ether, and the content of each component is shown in table 2 below.
Example 12
The difference from the example 1 is that the raw material of the viscosity-reducing type polycarboxylate superplasticizer further comprises octadecyl amine, and the content of each component is shown in the following table 2.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40 ℃, and stirring for 30min to obtain a heterocyclic product;
under the condition of a constant-temperature water bath at 90 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 5 by using a 30% NaOH solution; then cooling to 50 ℃, adding the prepared heterocyclic product, and stirring for 18 min; and adding octadecylamine, and continuing stirring for 30min to obtain the water reducing agent.
Example 13
The difference from example 12 is that the raw material of the viscosity-reducing polycarboxylate water reducer further comprises laureth, and the content of each component is shown in table 2 below.
A preparation method of a viscosity-reducing polycarboxylate superplasticizer comprises the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40 ℃, and stirring for 30min to obtain a heterocyclic product;
mixing octadecyl amine and laurinol polyether to obtain a straight chain mixture;
under the condition of a constant-temperature water bath at 90 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3 hours, continuously preserving heat for 1 hour, and adjusting the pH value to 5 by using a 30% NaOH solution; then cooling to 50 ℃, adding the prepared heterocyclic product, and stirring for 18 min; and adding the straight chain mixture, and continuously stirring for 30min to obtain the water reducing agent.
Example 14
The difference from the example 1 is that the raw material of the viscosity-reducing type polycarboxylate superplasticizer further comprises laureth, and the content of each component is shown in the following table 2.
Example 15
The difference from example 12 is that octadecylamine was replaced with aniline, and the contents of the respective components are shown in table 2 below.
Example 16
The difference from example 13 is that the laureth ether was replaced with diethyl ether and the contents of the respective components are shown in Table 2 below.
Comparative example
Comparative example 1
The difference from the example 1 is that the raw materials of the polycarboxylic acid water reducing agent are methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate, sodium methallyl sulfonate and an initiator, wherein the initiator is ammonium persulfate, and the content of each component is shown in the following table 1.
Comparative example 2
The difference from example 1 is that 3-oxetanone was replaced with acetophenone, and the contents of the components are shown in Table 1 below.
Comparative example 3
The difference from example 1 is that dimethyl sebacate was replaced by ethyl formate and the contents of the components are shown in table 1 below.
TABLE 1 component content tables of examples 1 to 6 and comparative examples 1 to 3
TABLE 2 ingredient content tables for examples 7-16
Performance test
(1) Testing viscosity reduction performance; the viscosity reduction performance is characterized by the fluidity of the neat paste, the cement used is M32.5 of Jinyuan cement Co., Ltd, Zhejiang according to GB 8077-; the higher the net pulp fluidity is, the higher the viscosity reduction degree is; the test results are shown in table 3 below.
TABLE 3 table of results of performance test of each example and comparative example
(2) Testing the compressive strength; limestone and river sand with the weight portion ratio of 4:1 are used as aggregate, the water reducing agent prepared by the preparation methods of the embodiments and the comparative examples is added, the using amount of the water reducing agent accounts for 5% of the aggregate, and a concrete test piece with the thickness of 100mm multiplied by 100mm is formed according to JTG E3-2005 Highway engineering cement and cement concrete test regulations; the compressive strength of the concrete test pieces cured for 1 day in example 1 and comparative example 1 was tested with reference to GB 8076-.
The test results are: the compressive strength of example 1 was 30.2 MPa; the compressive strength of the comparative example 1 is 24.9MPa, so that the viscosity-reducing polycarboxylate superplasticizer disclosed by the application also has a certain effect of improving the strength of concrete.
In summary, the following conclusions can be drawn:
1. according to the embodiment 1 and the embodiments 7 to 11 and the combination of the table 3, the respective addition of the 2-pyridineboronic acid and the glyceryl oleate has a promoting effect on the improvement of the viscosity reduction performance of the water reducing agent, and the joint addition of the two has a better effect of synergistically promoting the viscosity reduction performance of the water reducing agent.
2. According to example 1 and examples 12 to 16 in combination with Table 3, it can be seen that octadecylamine can improve the viscosity reduction effect of the water reducing agent, probably because octadecylamine has good space extension and shielding effects, and can hinder the accumulation and aggregation of cement particles; and the viscosity reduction performance of the water reducing agent can be further improved by mixing the laureth and the octadecylamine.
3. According to the example 1 and the comparative example 1 and the combination of the table 3, the water reducing agent prepared by the application has better viscosity reduction effect.
4. As can be seen from example 1 and comparative examples 2 to 3 in combination with Table 3, the co-addition of 3-oxetanone and dimethyl sebacate can improve the viscosity reduction performance of the water reducing agent, and the reason for this is probably that the mixed product of 3-oxetanone and dimethyl sebacate can diffuse into the cement particles with the addition of the water reducing agent, and is bonded with oily molecules through heterocyclic atoms, and the formation of complex between the cement particles is reduced by the special spatial configuration of 3-oxetanone, so that the aggregates of the cement particles are separated and the viscosity reduction is achieved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications to the present embodiment as necessary without inventive contribution after reading the present specification, but all are protected by patent law within the scope of the claims of the present application.
Claims (7)
1. The viscosity reduction type polycarboxylate superplasticizer is characterized by comprising the following components in parts by weight: the viscosity reduction type polycarboxylate superplasticizer comprises the following raw materials in parts by weight:
5-8 parts of methacrylic acid;
15-20 parts of acrylic acid;
2-3 parts of methoxy polyethylene glycol acrylate;
1-2 parts of sodium methallyl sulfonate;
1-2 parts of an initiator;
4-5 parts of 3-oxetanone;
1.5-2 parts of dimethyl sebacate;
40-50 parts of water, namely,
2-3 parts of 2-pyridine boric acid.
2. The viscosity reduction type polycarboxylate superplasticizer according to claim 1, characterized in that: the raw material also comprises 3-4 parts of glyceryl oleate according to parts by weight.
3. The viscosity reduction type polycarboxylate superplasticizer according to claim 1, characterized in that: the raw materials also comprise 1-2 parts of octadecylamine according to parts by weight.
4. The viscosity reduction type polycarboxylate superplasticizer according to claim 3, characterized in that: the raw materials also comprise 0.5 to 0.6 portion of laureth by weight.
5. The viscosity reduction type polycarboxylate superplasticizer according to claim 1, characterized in that: the initiator is ammonium persulfate.
6. The preparation method of the viscosity-reducing polycarboxylate superplasticizer according to claim 1, characterized by comprising the following steps:
mixing 3-oxetanone and dimethyl sebacate, heating to 40-45 ℃, and stirring for 30-40min to obtain a heterocyclic product;
under the condition of a thermostatic water bath at 90-95 ℃, mixing methacrylic acid, acrylic acid, methoxy polyethylene glycol acrylate and sodium methallyl sulfonate to obtain a mixed solution, then dropwise adding the mixed solution into water, dropwise adding an initiator, completing dropwise adding within 3-4h, continuously preserving heat for 1h, and adjusting the pH value to 5-6 by using a 30% NaOH solution; then cooling to 50-60 ℃, adding the prepared heterocyclic ring product, and stirring for 18-20min to obtain the water reducing agent.
7. The preparation method of the viscosity-reduction type polycarboxylate superplasticizer according to claim 6, which is characterized by comprising the following steps:
fully mixing 2-3 parts of 2-pyridine boric acid and 0.6-0.8 part of glyceryl oleate, heating to 30-40 ℃, and stirring for 15-25min to obtain a coordination mixture;
mixing 2-3 parts of octadecylamine and 0.5-0.6 part of laureth to obtain a straight-chain mixture;
adjusting pH to 5-6 with 30% NaOH solution, cooling to 50-60 deg.C, adding heterocyclic mixture obtained by stirring 4-5 parts of 3-oxetanone and 1.5-2 parts of dimethyl sebacate at 40-45 deg.C for 30-40min, and continuing stirring for 18-20 min; then adding the coordination mixture, and stirring for 20-25 min; and adding the straight chain mixture, and continuously stirring for 30-40min to obtain the water reducing agent.
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