CN114634327B - Pure lithium-based sealing curing agent and preparation method thereof - Google Patents

Pure lithium-based sealing curing agent and preparation method thereof Download PDF

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CN114634327B
CN114634327B CN202210228655.9A CN202210228655A CN114634327B CN 114634327 B CN114634327 B CN 114634327B CN 202210228655 A CN202210228655 A CN 202210228655A CN 114634327 B CN114634327 B CN 114634327B
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curing agent
lithium
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micro powder
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CN114634327A (en
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刘钦
王燕
王永
王海青
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Caparol China Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/60Agents for protection against chemical, physical or biological attack
    • C04B2103/603Agents for controlling alkali-aggregate reactions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/60Agents for protection against chemical, physical or biological attack
    • C04B2103/65Water proofers or repellants

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention belongs to the technical field of terrace materials, and relates to a pure lithium-based sealing curing agent and a preparation method thereof. The curing agent comprises: lithium silicate, active polymer modified composite metal inorganic micro powder, water and optional auxiliary agent; the particle surface of the active polymer modified composite metal inorganic micro powder is subjected to passivation and silane coupling agent treatment; the content of lithium element in the curing agent accounts for more than 85 mass percent of the total content of all metal elements, and preferably more than 90 mass percent. The curing agent only selects the lithium silicate as the main component, and is compounded with the composite metal inorganic micro powder modified by the active polymer, so that the defect of poor wear resistance of the concrete base layer constructed by the lithium silicate can be greatly improved. The sealing curing agent improves the wear resistance of a concrete ground or a wear-resistant aggregate terrace, does not return alkali, does not generate alkali-silicate reaction (ASR reaction), does not cause later expansion and cracking of concrete, and is the most excellent and ideal sealing curing agent at present.

Description

Pure lithium-based sealing curing agent and preparation method thereof
Technical Field
The invention belongs to the technical field of terrace materials, and particularly relates to a pure lithium-based sealing curing agent and a preparation method thereof.
Background
There are two main types of sealing and curing agents currently on the market. One class is silicate based sealing hardeners, representative of which are: the main components of the lithium-based sealing curing agent, the potassium-based sealing curing agent and the sodium-based sealing curing agent are respectively lithium silicate, sodium silicate and potassium silicate, the reaction equation of the lithium-based sealing curing agent, the potassium-based sealing curing agent and the sodium-based sealing curing agent with the cement hydration by-product calcium hydroxide is shown in the specification,
Li 2 SiO 3 +Ca(OH) 2 →CaSiO 3 ↓+2LiOH
K 2 SiO 3 +Ca(OH) 2 →CaSiO 3 ↓+2KOH
Na 2 SiO 3 +Ca(OH) 2 →CaSiO 3 ↓+2NaOH
the generated alkali-insoluble strong base weak acid salt (in alkaline state) precipitates and is filled in the gaps of the concrete in a gel state.
Another class of seal hardeners are the fluorosilicates, represented by magnesium fluorosilicate, which react with the calcium hydroxide byproduct of cement hydration in the following equation
MgSiF 6 +2Ca(OH) 2 →MgF 2 ↓+2CaF 2 ↓+SiO 2 +2H 2 O
Ca(OH) 2 +SiO 2 +H 2 O→C-S-H
Magnesium fluosilicate and Ca (OH) 2 Insoluble matter (MgF) formed 2 And CaF 2 And C-S-H gel) are filled in the gaps of the cement base body, so that the cement base material is more compact.
However, magnesium fluorosilicate contains a small amount of magnesium sulfate and fluorosilicic acid. Fluorosilicic acid is extremely toxic and can attack mucous membranes, eyes and skin. During the use process, hydrogen fluoride is generated, and fluorine ions are combined with calcium ions to influence the nerve function and seriously reduce the bone density to cause bone complications. The reaction equation is as follows
MgSiF 6 +2Ca(OH) 2 →MgF 2 ↓+2CaF 2 ↓+SiO 2 +2H 2 O
MgF 2 ↓+H + →Mg 2 ++2HF↑
In 1940, stanton found ASR Reaction, alkali Silica Reaction (Alkali-Silica Reaction). By 1957 Swenson discovered an ACR Reaction, i.e., an Alkali carbonate Reaction (Alkali-carbonate Reaction). Both of these general classes of reactions are actually attributed to the alkali-aggregate reaction (AAR). The alkali-aggregate reaction (AAR), known as the "cancer" of concrete, poses a great hazard to concrete engineering, and is currently avoided in various ways. The reaction of sodium silicate and potassium silicate with concrete belongs to active alkali-silicon reaction, and potassium-based and sodium-based hardeners generate a product (C-N (K) -S-H gel) with the property of water swelling, so that concrete structures are easy to crack.
Na + (K + )+Ca 2+ +SiO 2 +OH - →C-N(K)-S-H (1)
N(K)-S-H(l)+H 2 O→C-N(K)-S-H (2)
The lithium-based sealing curing agent can effectively inhibit the alkali aggregate reaction and play a role in repairing, so that the size of the concrete is kept stable.
Li + +SiO 2 +OH - →L-S-H (1)
The lithium silicate gel L-S-H is preferentially generated, and Na can be prevented + 、K + Erosion of aggregate;
Na + (K + )+Ca 2+ +SiO 2 +OH - →C-N(K)-S-H (2)
C-N(K)-S-H(l)+H 2 O+Li + →L-S-H+Na + (K + ) (3)
alkali silicate gel, li, already formed + Can be substituted for Na + 、K + So that it loses its swelling destructive action. The lithium silicate gel L-S-H is colorless liquid and is a non-swelling substance, and does not generate swelling damage to the system. The dehydrated solid lithium silicate has compact structure, can effectively fill concrete gaps, and plays a role in reinforcement. In view of the advantages and disadvantages of the above-mentioned types of permeable liquid hardeners, lithium-based liquid hardeners are undoubtedly the last choice.
However, the ground mode hardness of the lithium-based concrete sealing and curing agent can only reach 6-7 generally, and the ground mode hardness of the sodium-based or potassium-based concrete sealing and curing agent can reach 7-9. Obviously, the pure lithium-based sealing curing agent is slightly inferior to a sodium-based or potassium-based sealing curing agent in wear resistance, so that pure lithium is used as a main component in the market and can achieve very little excellent wear resistance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a pure lithium-based sealing curing agent which is not compounded with sodium silicate, potassium silicate and the like, has no toxicity, environmental protection and extremely high surface wear resistance, and is suitable for various cement-based terraces.
In order to achieve the above object, a first aspect of the present invention provides a pure lithium-based sealing curing agent, comprising: lithium silicate, active polymer modified composite metal inorganic micro powder, water and optional auxiliary agent; the particle surface of the active polymer modified composite metal inorganic micro powder is subjected to passivation and silane coupling agent treatment; the content of lithium element in the curing agent accounts for more than 85 mass percent of the total content of all metal elements, and preferably more than 90 mass percent.
The second aspect of the invention provides a preparation method of a pure lithium-based sealing curing agent, which comprises the following steps:
1) Mixing lithium silicate and composite metal inorganic micro powder modified by active polymer and primarily dispersing to obtain a mixture;
2) And dispersing the mixture, water and optional auxiliary agent again to obtain the pure lithium-based sealing curing agent.
The strength of concrete is mainly derived from calcium silicate compounds (C-S-H) generated by silicon and calcium in cement components in the concrete under the action of water, and the C-S-H is a substance playing a main strength role in the concrete. The slow C-S-H hydration reaction inside the concrete still continues after the initial setting of the concrete, the reaction can not completely proceed under natural conditions, and a large amount of free calcium, ca and the like always exist 2+ No generation of active Silicate Ion (SiO) contained in the C-S-H lithium-based curing agent 3 2- ). By effective penetration, the active silicon reacts with free calcium (Ca) in the concrete which has not reacted to calcium silicate 2+ ) Calcium ions react to form calcium silicate hydrate (C-S-H), so that calcium ions in the concrete further participate in the reaction (the reaction lasts for about 60 to 90 days) to form a permanent gel. A network structure is formed in three-dimensional space, and a compact and firm whole is formed. Therefore, the concrete can be compacted, the excellent quality is shown in the aspects of improving the integral surface strength, the wear resistance, the seepage prevention, the dust prevention, the sand prevention, the skid resistance and the ageing resistance of the concrete, and the service life of the concrete is prolonged. Lithium-based sealingThe addition of the agent can effectively inhibit the reaction of the alkali aggregate and play a role in repairing, so that the size of the concrete is kept stable.
Therefore, the beneficial effects of the invention are as follows:
1) The lithium-based concrete has better permeability than potassium-based and sodium-based concrete
The stronger the alkalinity is, the faster the reaction rate is, the more violent the reaction of the sodium silicate and the potassium silicate is, the faster the gel of C-S-H is formed, so the capillary pores of the concrete surface layer can be quickly compacted, and the extending and the penetration of the curing agent to the depth direction can be prevented. Lithium silicate is less basic, forming C-S-H gels slower, and the material penetrates deeper (5-8 mm). The deep penetration of the material is larger in the participating reaction bonding layer. Further, lithium has a much smaller degree of polymerization and molecular weight than potassium and sodium. Also, the same amount of Na + Silicon dioxide, K + Silicon dioxide, li + Silicon dioxide. Apparent Li + More silica was carried in and more C-S-H gel was formed. Inside the concrete, the three-dimensional network space forms a compact whole, which is larger and more compact.
2) The lithium-based concrete sealing curing agent has good water resistance
The lithium silicate has water irreversibility, potassium-based and sodium-based ground surfaces, is not water-resistant and is easy to lose light after being soaked in water. The lithium base has good dry and wet alternation resistance, and does not have images in a highly humid environment in time.
3) The glossiness of the lithium-based concrete sealing curing agent is better
The terrace made by the sodium-based concrete sealing curing agent or the potassium-based concrete sealing curing agent has hazy and unclear glossiness, the lithium-based sealing curing agent can be obviously different, and the made floor has transparent feeling. The more the lithium-based concrete is used, the brighter it is, and the later physical friction, such as rolling with wheels, mopping back and forth, etc., which naturally rubs, the more brightly it is used over time.
4) The lithium-based concrete does not generate efflorescence
The sodium-based or potassium-based sealing curing agent has strong alkalinity, and when the effective components in the material are permeated and react with free calcium in concrete to form a calcium silicate compound, a byproduct strong base can be formed, and the strong base can be brought out of the water surface by the free water. After being brought out of the water, it reacts with carbon dioxide in the air. White substances attached to the surface of concrete are formed, and are commonly called whiskering. Lithium-based curing agents do not produce this phenomenon.
5) Lithium-based concrete sealing curing agent has no ASR reaction (alkali-silicate reaction)
The ASR reaction is one of the AAR reactions (alkali-aggregate reaction). It is called a cancer of concrete, due to the erosion of aggregates by alkali, forming an alkali-silicic acid gel. The sodium-based potassium has strong hydrophilicity. It is easy to absorb water from air and concrete, causing the system to expand, and further causing cracks in the concrete. The lithium-based curing agent is relatively stable, does not absorb water, and does not expand even in a high-strength environment, so that the lithium-based material does not cause cracking.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
The invention provides a pure lithium-based sealing curing agent, which comprises the following components: lithium silicate, active polymer modified composite metal inorganic micro powder, water and optional auxiliary agent; the particle surface of the active polymer modified composite metal inorganic micro powder is subjected to passivation and silane coupling agent treatment; the content of lithium element in the curing agent accounts for more than 85 mass percent of the total content of all metal elements, and preferably more than 90 mass percent. The pure lithium-based sealing curing agent does not contain sodium silicate and potassium silicate.
According to the invention, the curing agent comprises the following raw materials in parts by weight:
Figure BDA0003537293290000051
optionally, the auxiliary agent is at least one selected from a defoaming agent, a wetting agent and an anti-permeability agent, and the auxiliary agents comprise the following components in parts by weight:
0-1.5 parts of defoaming agent, preferably 0.1-1.5 parts;
0-2 parts of wetting agent, preferably 0.1-2 parts;
0-2 parts of anti-permeability agent, preferably 0.1-2 parts.
Specifically, the modulus of the lithium silicate is 2 to 5, preferably 2.5 to 4.8.
According to the invention, the active polymer modified composite metal inorganic micro powder is alkaline and has a pH =8-10.
Specifically, the active polymer modified composite metal inorganic micro powder is prepared by performing surface coating passivation treatment and silane coupling agent treatment on mineral micro powder, and preferably, the active polymer modified composite metal inorganic micro powder is selected from at least one of coated micro powder MP001, MP003 and MP 004.
The active polymer modified composite metal inorganic micro powder MP001, MP-003 and MP-004 used in the invention is composite mineral micro powder, and the main components of the composite mineral micro powder are as follows: zinc oxide (ZnO) and aluminum oxide (Al) 2 O 3 ) Titanium dioxide (TiO) 2 ) And the like. The final grading proportion is calculated by utilizing mineral structures with different forms (the forms of the mineral structures have similar spherical shapes, needle shapes, sheet shapes and the like), and then special coating passivation treatment and silane coupling agent (active polymer of lithium silicate) treatment are carried out on the surface of the mineral micro powder with strong reactivity to obtain the active polymer modified composite metal inorganic micro powder.
The molecular structural formula of the silane coupling agent is Y-R-Si (OR) 3 (wherein Y-organic functional group, siOR-siloxy). The siloxy group is reactive with lithium silicate and the organofunctional group is reactive or compatible with organics. Thus, when a silane coupling agent intervenes between the inorganic and organic interfaces, a bonding layer of organic matrix-silane coupling agent-inorganic matrix may be formed.
The composite metal inorganic micro powder modified by the active polymer adopts a passivation process, effectively reduces the dissociation quantity in the multivalent electrolyte water, and solves the post-thickening problem of lithium silicate; the polymer is modified, so that the crosslinking property between the polymer and lithium silicate in a film forming stage is improved, and the problems of coating powder falling and water resistance are solved; has high wear resistance and weather resistance, and can be easily dispersed in water.
The reaction mechanism of the active polymer modified composite metal inorganic micro powder is as follows: the composite metal inorganic micro powder modified by the active polymer is equivalent to a latent curing agent, and when the composite metal inorganic micro powder is dispersed in water, no reaction occurs due to the polymerization inhibition effect of the water, and the water acts as a polymerization inhibitor. However, after the water is evaporated, a special curing reaction with lithium silicate occurs, namely, cross-linking coupling is generated, and the abrasion resistance, the water resistance and the film forming property are increased. The main reaction equation is as follows:
Li 2 O·nSiO 2 +M(OH) 2 →MO·SiO 2 +(n-1)SiO 2 +2LiOH
2LiOH+CO 2 →Li 2 CO 3 +H 2 O
in the formula: m = Zn, al or other active metal, the presence of which initiates the solidification reaction of lithium silicate, making the reaction more complete and the film formation more excellent.
The reaction activity sequence of the coated micro powder used in the invention is MP001 > MP-003 > MP-004.
Specifically, the defoaming agent is selected from at least one of a silicone defoaming agent and a mineral oil defoaming agent;
the wetting agent is at least one of glycerol and triethanolamine.
According to the invention, the anti-permeability agent is preferably an oligomeric propylsilicate.
The invention also provides a preparation method of the pure lithium-based sealing curing agent, which comprises the following steps:
1) Mixing lithium silicate and composite metal inorganic micro powder modified by active polymer and primarily dispersing to obtain a mixture;
2) And dispersing the mixture, water and optional auxiliary agent again to obtain the pure lithium-based sealing curing agent.
Optionally, the conditions of the preliminary dispersion include: the rotating speed is 300-1000 r/min, preferably 500-800 r/min; the time is 15-25 min, preferably 18-22min;
the conditions for re-dispersion include: the rotating speed is 300-1000 r/min, preferably 500-800 r/min; the time is 5-15 min, preferably 8-12min.
The present invention is explained in more detail by examples, comparative examples and test examples.
In the following examples and comparative examples, the components were obtained commercially.
The active polymer modified composite metal inorganic micro powder is coating micro powder MP001, MP003 and MP004 of Shanghai Wabeis new material company Limited;
silicone defoamer is byk 024, birk chemical;
the wetting agent is glycerol, nanjing A-B-Xin-Wei chemical Co., ltd;
the anti-permeability agent is propyl orthosilicate, hydrophobic lotus leaf effect, protecosil ws 808, EVONIC (winning chemistry);
in distinction to alkali metal silicate solutions: the alkali metal silicate solution mentioned in part of the resin system refers to a composite solution of potassium silicate, sodium silicate and lithium silicate, the combination of which lacks formulation design and cannot meet the requirements of JC/T2158-2021.
Comparative example 1
The existing lithium-based sealing curing agent on the market is selected and purchased.
Comparative example 2
70 parts by weight of lithium silicate (Xian' tong xin TX-L35) is mixed and dispersed with 0.5 part by weight of organic silicon defoamer, 1 part by weight of wetting agent, 1 part by weight of anti-permeability agent and 30 parts by weight of water, the dispersion speed is 300-1000 r/min, and the dispersion time is 10-25 min. Dispersing to obtain the pure lithium-based sealing curing agent.
Example 1
This example illustrates the preparation of a pure lithium-based sealing hardener according to the invention.
Mixing 70 parts by weight of lithium silicate (Xian Tongxin TX-L35), 0.5 part of coated micro powder MP001 and 0.5 part of coated micro powder MP003, and dispersing at the rotating speed of 300-1000 r/min for 10-25 min; adding 0.5 weight part of organic silicon defoaming agent, 1 weight part of wetting agent, 1 weight part of anti-permeability agent and 30 weight parts of water into the mixture, wherein the dispersion rotating speed is 300-1000 r/min, and the dispersion time is 5-20 min. Dispersing to obtain the pure lithium-based sealing curing agent.
Example 2
This example illustrates the preparation of a pure lithium-based sealing hardener according to the invention.
70 parts by weight of lithium silicate (Xian Tongxin TX-L35), 0.5 part of coated micro powder MP001 and 0.5 part of coated micro powder MP004 are mixed and dispersed, the dispersion rotating speed is 300-1000 r/min, and the time is 10-25 min; adding 0.5 weight part of organic silicon defoaming agent, 1 weight part of wetting agent, 1 weight part of anti-permeability agent and 30 weight parts of water into the mixture, wherein the dispersion rotating speed is 300-1000 r/min, and the dispersion time is 5-20 min. Dispersing to obtain the pure lithium-based sealing curing agent.
Example 3
This example illustrates the preparation of a pure lithium-based sealing hardener according to the invention.
70 parts by weight of lithium silicate (Xian Tongxin TX-L35) and 0.5 part of coated micro powder MP001 are mixed and dispersed, the dispersion rotating speed is 300-1000 r/min, and the time is 10-25 min; adding 0.5 weight part of organic silicon defoaming agent, 1 weight part of wetting agent, 1 weight part of anti-permeability agent and 30 weight parts of water into the mixture, wherein the dispersion rotating speed is 300-1000 r/min, and the dispersion time is 5-20 min. Dispersing to obtain the pure lithium-based sealing curing agent.
Test example 1
The commercially available lithium-based sealing hardener of comparative example 1 was subjected to the standard JC/T2158-2021 test, and the test results are shown in Table 1.
TABLE 1
Figure BDA0003537293290000091
Figure BDA0003537293290000101
As can be seen from Table 1, comparative example 1 does not meet all of the test items in the Roche JC/T2158-2021. Wherein, the abrasion resistance is not tested because the base layer is abraded, so the data is not available and the product is not qualified. The surface hardness was also unsatisfactory, 5mm, and the surface water absorption capacity was also relatively high, 4, indicating insufficient densification.
Test example 2
The pure lithium-based sealing curing agent prepared in comparative example 2 was subjected to the line code JC/T2158-2021 test, and the test results are shown in Table 2.
TABLE 2
Figure BDA0003537293290000102
As can be seen from Table 2, comparative example 2 does not meet all of the test items in the Row code JC/T2158-2021. Wherein, the abrasion resistance is that the base layer is abraded and can not be tested, so that no data exists, and the product is unqualified. The surface hardness was also found to be 6mm. This shows that the wear resistance of pure lithium silicate is relatively poor, and the surface wear resistance is difficult to reach the standard by using the lithium silicate as the main gel material.
Test example 3
The pure lithium-based sealing curing agent prepared in example 1 was subjected to the line code JC/T2158-2021 test, and the test results are shown in Table 3.
TABLE 3
Serial number Inspection item JC/T 2158-2021 Example 1
1 Appearance of the product Transparent, homogeneous liquid Transparent, homogeneous liquid
2 Solids content Numerical value. + -. 2 23%
3 pH value ≥10 11.9
4 24h surface water absorption capacity mm ≤5 1
5 Viscosity of the oil 1~10mpa s 5.9
6 Abrasion resistance/mm ≤0.2 0.07
7 Surface hardness ≤4.5 4.3
8 voc ≤20 Not detected out
9 Whether or not the excessive accumulation of alkali is whitish - Whether or not
As can be seen from Table 3, the seal hardeners of the present invention fully meet all the test items in the line code JC/T2158-2021. Among them, the abrasion resistance was 0.07mm. The surface hardness was also high, and was 4.3mm. Because of being pure lithium base, the crystal has no phenomenon of alkali reversion and whitening. The pH was 11.9, and the sealing agent was alkaline. The 24h surface water absorption capacity is 1mm, which shows that the impermeability is good and the density is relatively high.
Test example 4
The pure lithium-based sealing curing agent prepared in example 2 was subjected to the line code JC/T2158-2021 test, and the test results are shown in Table 4.
TABLE 4
Serial number Inspection item JC/T 2158-2021 Example 2
1 Appearance of the product Transparent, homogeneous liquid Transparent, homogeneous liquid
2 Solids content Numerical value. + -. 2 22%
3 pH value ≥10 11.6
4 24h surface water absorption capacity mm ≤5 1.5
5 Viscosity of the oil 1~10mpa s 5.5
6 Abrasion resistance/mm ≤0.2 0.1
7 Surface hardness ≤4.5 4.4
8 voc ≤20 Not detected out
9 Whether or not the excessive accumulation of alkali is whitish - Whether or not
As can be seen from Table 4, the seal curing agent of the present invention completely met all test items in the Row code JC/T2158-2021. Wherein the abrasion resistance is 0.1mm. The surface hardness was also high, and was 4.4mm. Because of being pure lithium base, the crystal has no phenomenon of alkali reversion and whitening. The pH was 11.6, and the sealing agent was alkaline. The water absorption capacity of the surface is 1.5mm after 24 hours, which shows that the impermeability is good and the surface is compact.
Test example 5
The pure lithium-based sealing curing agent prepared in example 3 was subjected to the line code JC/T2158-2021 test, and the test results are shown in Table 5.
TABLE 5
Figure BDA0003537293290000121
Figure BDA0003537293290000131
As can be seen from Table 5, the seal hardeners of the present invention fully meet all the test items in the line code JC/T2158-2021. Among them, the abrasion resistance was as good as 0.12mm. The surface hardness was also high, and was 4.4mm. Because of being pure lithium base, the crystal has no phenomenon of alkali reversion and whitening. The pH was 11.4, and the sealing agent was alkaline. The 24h surface water absorption capacity is 2mm, which shows that the impermeability is good and the density is relatively high.
Test example 6
To further illustrate, the lithium content in the curing agent of example 1 and example 2 was analyzed by ICP-OES element analysis by Shanghai organic chemistry research institute of academy of sciences, and the test results are shown in Table 6.
TABLE 6
Figure BDA0003537293290000132
From the elemental analysis in table 6, the lithium content is defined as the lithium element divided by the total metal element content, the lithium element accounts for 90% or more, and a small amount of sodium element is considered to be present as a stabilizer in the raw material, and the remaining elements are small in amount. It can be seen that the lithium content is already very high and can be considered as a pure lithium-based curing agent.
In order to more clearly demonstrate the performance of the sealing hardeners of the present invention, the data in test examples 1-5 are summarized in Table 7.
TABLE 7 COMPARATIVE EXAMPLES AND COMPARATIVE EXAMPLES
Figure BDA0003537293290000141
From the comparative data in table 7, it can be seen that the properties of example 1 are most excellent. In terms of abrasion resistance, example 1 had an abrasion resistance of 0.07mm, and examples 2 and 3 were also acceptable but lower than example 1, while comparative example 2 was not acceptable due to abrasion of the base layer. The same rule is also shown in terms of surface hardness, with example 1 being the best and 4.2mm, example 2 being 4.4mm and 4.5mm in criticality compared to example 3 and comparative example 2 being 6mm, failing. In terms of surface water absorption, example is 1mm, most preferred, example 2 is similar to example 3, and comparative example 2 is worst. Comparative example 1 is similar to comparative example 2 in that the base layer is abraded, no wear resistance data exists, the surface hardness is unqualified, the surface water absorption capacity is high, and the situation is not compact enough.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.

Claims (12)

1. A pure lithium-based sealing curative, comprising: lithium silicate, active polymer modified composite metal inorganic micro powder, water and optional auxiliary agent;
the particle surface of the active polymer modified composite metal inorganic micro powder is subjected to passivation and silane coupling agent treatment;
the content of lithium element in the curing agent accounts for more than 85 mass concentration percent of the total content of all metal elements;
the active polymer modified composite metal inorganic micro powder is alkaline, and the pH =8-10;
the active polymer modified composite metal inorganic micro powder is prepared by performing surface coating passivation treatment and silane coupling agent treatment on mineral micro powder;
the active polymer modified composite metal inorganic micro powder is selected from at least one of coating micro powder MP001, MP003 and MP004;
the active polymer modified composite metal inorganic micro powder comprises the following components: zinc oxide, aluminum oxide and titanium dioxide.
2. The pure lithium-based sealing curing agent according to claim 1, wherein the content of lithium element in the curing agent is 90 mass% or more based on the total content of all metal elements.
3. The pure lithium-based sealing curing agent according to claim 2, wherein the curing agent comprises the following raw materials in parts by weight:
50-100 parts of lithium silicate;
0.1-5 parts of active polymer modified composite metal inorganic micro powder;
1-50 parts of water;
0-8 parts of an auxiliary agent.
4. The pure lithium-based sealing curing agent according to claim 3, wherein the auxiliary agent is at least one selected from an antifoaming agent, a wetting agent and an anti-permeation agent, and the weight parts of each auxiliary agent are as follows:
0-1.5 parts of a defoaming agent;
0-2 parts of a wetting agent;
0-2 parts of an anti-permeability agent.
5. The pure lithium-based sealing curing agent according to claim 4, wherein the weight parts of each auxiliary agent are as follows:
0.1-1.5 parts of defoaming agent;
0.1-2 parts of a wetting agent;
0.1-2 parts of an anti-permeability agent.
6. The pure lithium based sealing and curing agent according to any one of claims 1 to 5, wherein the module of the lithium silicate is 2 to 5.
7. The pure lithium based sealing and curing agent according to claim 5, wherein the modulus of the lithium silicate is 2.5 to 4.8.
8. The pure lithium-based sealing curing agent according to any one of claims 4 to 5, wherein the defoamer is at least one selected from silicone defoamers, mineral oil defoamers;
the wetting agent is at least one of glycerol and triethanolamine.
9. The pure lithium-based sealing and curing agent according to any one of claims 4 to 5, wherein the permeation resistant agent is propyl oligosilicate.
10. The method for preparing a pure lithium-based sealing curing agent according to any one of claims 1 to 9, comprising the steps of:
1) Mixing lithium silicate and composite metal inorganic micro powder modified by active polymer and primarily dispersing to obtain a mixture;
2) And dispersing the mixture, water and optional auxiliary agent again to obtain the pure lithium-based sealing curing agent.
11. The production method according to claim 10, wherein the conditions for the preliminary dispersion include: the rotating speed is 300 to 1000r/min; the time is 15 to 25min;
the conditions for re-dispersion include: the rotating speed is 300 to 1000r/min; the time is 5 to 15min.
12. The method of claim 11, wherein the conditions for the preliminary dispersion include: the rotating speed is 500 to 800r/min; the time is 18-22min;
the conditions for re-dispersion include: the rotating speed is 500 to 800r/min; the time is 8-12min.
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