CN108046690B - Preparation method of high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive - Google Patents
Preparation method of high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive Download PDFInfo
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- CN108046690B CN108046690B CN201711246563.9A CN201711246563A CN108046690B CN 108046690 B CN108046690 B CN 108046690B CN 201711246563 A CN201711246563 A CN 201711246563A CN 108046690 B CN108046690 B CN 108046690B
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/18—Lignin sulfonic acid or derivatives thereof, e.g. sulfite lye
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/38—Polysaccharides or derivatives thereof
- C04B24/383—Cellulose or derivatives thereof
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00637—Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials
Abstract
The invention relates to the technical field of preparation of reinforcing materials for building structures, in particular to a preparation method of a high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive. The invention takes straws as raw materials, and the straws are heated and boiled to obtain lignin alkali liquor, the lignin alkali liquor is neutralized by acetic acid, and then is subjected to high-speed centrifugation, washing and drying to obtain lignin powder, a self-made solid crude product is treated to obtain white powder, and diluted slurry is mixed with the lignin powder, quartz sand, fly ash and the like to prepare the inorganic reinforcing steel bar anchoring adhesive.
Description
Technical Field
The invention relates to the technical field of preparation of reinforcing materials for building structures, in particular to a preparation method of a high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
Background
The anchoring adhesive is commonly called as bar planting adhesive and is mainly used for enhancing the connection between concrete and steel bars in the building industry. The reinforced concrete structure occupies an extremely important position and a considerable amount in the buildings in China, and with the development of economic construction and industrial structure in China, the anchor adhesive is rapidly developed and widely applied in recent years.
Commonly used reinforcing steel anchoring materials are classified into organic and inorganic materials. The organic anchoring material is generally made of epoxy-based structural adhesive, although the strength is high, the water resistance is poor, the bonding strength is low in a humid environment, the organic anchoring material is easy to age in an ultraviolet irradiation environment, the difference between the linear expansion coefficient of the organic anchoring material and the linear expansion coefficient of concrete is too large, the organic anchoring material is easy to deform and peel, and the raw materials contain more toxic or slightly toxic components, so that the organic anchoring material is easy to damage human bodies and pollute the environment.
At present, the inorganic anchoring adhesive in the market mainly comprises silicate cement or sulphoaluminate cement compounded with various functional additives, admixtures and inorganic fillers, has the characteristics of quick setting, quick hardening, fire resistance, high shear strength, water resistance and the like, can be constructed by cold operation, and has no pollution to the environment. The anchor rod is mainly used for rapid construction of supporting surrounding rocks by the anchor rod for underground engineering such as railways, tunnels, house earthquake resistance, metallurgical mines and the like, and anchoring of the traction nail in concrete structure reinforcement engineering, and can meet the requirement of welding of steel bars. However, inorganic anchoring adhesives also have drawbacks such as: the bond strength is not high enough, part of the inorganic anchoring adhesive can show certain contractibility in the later period, the adhesive force between the adhesive and the concrete or steel is weak, and the adhesive strength between the adhesive and the base material concrete under the condition of constrained drawing is unstable. The popularization and the application of the inorganic adhesive in the concrete structure reinforcing engineering are limited to a certain extent.
Therefore, it is necessary to develop an inorganic reinforcing bar anchor adhesive that can solve the above performance problems.
Disclosure of Invention
The invention mainly solves the technical problem and provides a preparation method of a high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive aiming at the defect that the bonding force between the inorganic reinforcing steel bar anchoring adhesive and a reinforcing steel bar is weakened because the inorganic reinforcing steel bar anchoring adhesive shrinks at the later solidification stage.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive is characterized by comprising the following specific preparation steps:
(1) putting 200-230 g of straw residues and 400-450 mL of sodium hydroxide solution into a water bath reaction kettle with a stirrer, heating in a water bath, starting the stirrer to stir until the straw residues are completely dissolved to obtain lignin alkali liquor;
(2) neutralizing a lignin alkali liquor to be neutral by using glacial acetic acid to obtain a lignin suspension, placing the lignin suspension in a high-speed centrifuge for high-speed centrifugation, removing supernatant, separating to obtain lower-layer precipitate, washing the precipitate with water for 2-3 times, placing in an oven, and drying to obtain lignin powder;
(3) adding 70-75 g of beta-cyclodextrin and 100-130 mL of sodium hydroxide solution into a beaker, stirring at room temperature, adding 5-10 g of epoxypropyl trimethyl ammonium chloride, placing the beaker in a water bath kettle, heating, carrying out heat preservation reaction, and filtering to remove filtrate to obtain a solid crude product;
(4) dissolving the solid crude product with 200-250 mL of hot water, adjusting the pH value with dilute hydrochloric acid to obtain a neutralized solution, placing the neutralized solution in a vacuum drying oven, drying, and then placing in a mortar for grinding to obtain dry powder;
(5) dissolving 50-55 g of dry powder by using 200-220 mL of DMF (dimethyl formamide) solution to obtain a DMF solution, adding 150-170 mL of acetone into the DMF solution to obtain white powder slurry, performing suction filtration on the white powder slurry to remove filtrate and separate to obtain a product, placing the product in a vacuum drying oven, and drying to obtain white powder;
(6) adding 10-15 parts by weight of methyl allyl polyoxyethylene ether, 5-7 parts by weight of polyacrylamide and 80-90 parts by weight of distilled water into a stirrer, heating to raise the temperature, adding 20-30 parts by weight of lignin powder, 5-10 parts by weight of ammonium persulfate solution and 10-15 parts by weight of sodium sulfite solution into the stirrer, carrying out heat preservation reaction, cooling to room temperature, adding 70-80 parts by weight of ordinary portland cement, 20-25 parts by weight of fly ash, 10-15 parts by weight of magnesia and 20-25 parts by weight of white powder, and stirring and mixing to obtain the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
The mass fraction of the sodium hydroxide solution in the step (1) is 45%, the temperature is 90-95 ℃ after water bath heating, and the stirring time is 3-5 h.
The mass fraction of the glacial acetic acid in the step (2) is 95%, the rotating speed of a high-speed centrifuge is 3500-3700 r/min, the high-speed centrifugation processing time is 12-15 min, the set temperature of an oven is 70-80 ℃, and the drying time is 4-5 h.
And (3) the mass fraction of the sodium hydroxide solution in the step (3) is 90%, the stirring time is 10-15 min, the temperature after heating and temperature rise is 50-55 ℃, and the heat preservation reaction time is 3-4 h.
The temperature of the hot water in the step (4) is 60-65 ℃, the mass fraction of the dilute hydrochloric acid is 10%, the pH value of the dilute hydrochloric acid is adjusted to 6-7, the set temperature of the vacuum drying oven is 80-90 ℃, the drying time is 3-4 h, and the grinding time in a mortar is 3-4 h.
And (5) setting the temperature of the vacuum drying oven to be 80-90 ℃, and drying for 4-5 hours.
And (3) after heating and temperature rising, the temperature is 50-55 ℃, the mass fraction of the ammonium persulfate solution is 20%, the mass fraction of the sodium sulfite solution is 30%, the reaction time is 3-4 h, and the stirring speed is 80-85 r/min.
The invention has the beneficial effects that:
(1) the invention takes waste straws as raw materials, the waste straws are heated and boiled to obtain lignin alkali liquor, the lignin alkali liquor is neutralized by acetic acid, high-speed centrifugation, washing and drying are carried out to obtain lignin powder, beta-cyclodextrin is alkalized and then epoxypropyltrimethylammonium chloride is added for heating reaction and then filtration is carried out to obtain a solid crude product, the solid crude product is dissolved by hot water, white powder is obtained after neutralization, grinding and recrystallization purification, methyl allyl polyoxyethylene ether, polyacrylamide and distilled water are prepared to obtain diluted slurry, then the lignin powder and inorganic main materials such as quartz sand, fly ash and the like are added to obtain the inorganic reinforcing steel bar anchoring adhesive, the white powder in the invention is purified quaternary ammonium type cationic cyclodextrin, a small amount of quaternary ammonium type cationic cyclodextrin coats silicate cement in the anchoring adhesive in a colloid form in water, the quaternary ammonium cationic cyclodextrin repels cations on the surface of metal silicate in concrete, after the anchoring adhesive is rapidly solidified to bond the reinforcing steel bar, the quaternary ammonium cationic cyclodextrin permeates into the anchoring adhesive at the later stage of solidification to cause silicate cement particles in the anchoring adhesive to mutually repel each other, so that the shrinkage of the anchoring adhesive is reduced, and the bonding force between the inorganic reinforcing steel bar anchoring adhesive and the reinforcing steel bar is improved;
(2) the lignin recovered from the straw residues is used as a modified substance of the inorganic reinforcing steel bar anchoring adhesive, the lignin has a larger spatial structure, larger steric hindrance can be generated in the inorganic reinforcing steel bar anchoring adhesive, the improvement of the dispersion performance of the inorganic reinforcing steel bar anchoring adhesive is facilitated, the added sodium sulfite and the lignin are subjected to sulfonation reaction, sulfonic acid groups are introduced into lignin molecules, the hydrophilic performance of the inorganic reinforcing steel bar anchoring adhesive can be improved, the high dispersion of the reinforcing steel bar anchoring adhesive can be kept before solidification, the uniform density of each area of the inorganic reinforcing steel bar anchoring adhesive is kept, the shrinkage in the later solidification period is reduced, in addition, a certain amount of lignin is added, the average molecular weight of the inorganic reinforcing steel bar anchoring adhesive can be increased, the deposition density of the anchoring adhesive on the surface of a reinforcing steel bar is improved, the shrinkage in the rapid solidification of the inorganic reinforcing steel bar anchoring adhesive is reduced, and the cohesive force between the inorganic reinforcing steel, has wide application prospect.
Detailed Description
Putting 200-230 g of straw residues and 400-450 mL of 45% sodium hydroxide solution in a water bath reaction kettle with a stirrer, heating in a water bath to 90-95 ℃, starting the stirrer, and stirring for 3-5 hours until the straw residues are completely dissolved to obtain lignin alkali liquor; neutralizing a lignin alkali liquor to be neutral by using glacial acetic acid with the mass fraction of 95% to obtain a lignin suspension, placing the lignin suspension in a high-speed centrifuge, centrifuging at a high speed of 3500-3700 r/min for 12-15 min, removing the supernatant, separating to obtain a lower-layer precipitate, washing the precipitate with water for 2-3 times, placing in an oven with the set temperature of 70-80 ℃, and drying for 4-5 h to obtain lignin powder; adding 70-75 g of beta-cyclodextrin and 100-130 mL of 90% sodium hydroxide solution by mass into a beaker, stirring for 10-15 min at room temperature, then adding 5-10 g of epoxypropyl trimethyl ammonium chloride, placing the beaker into a water bath kettle, heating to 50-55 ℃, carrying out heat preservation reaction for 3-4 h, and filtering to remove filtrate to obtain a solid crude product; dissolving the solid crude product with 200-250 mL of hot water at the temperature of 60-65 ℃, adjusting the pH to 6-7 with 10% by mass of dilute hydrochloric acid to obtain a neutralized liquid, drying the neutralized liquid in a vacuum drying oven at the set temperature of 80-90 ℃ for 3-4 h, and grinding the dried liquid in a mortar for 3-4 h to obtain dry powder; dissolving 50-55 g of dry powder by using 200-220 mL of DMF (dimethyl formamide) solution to obtain a DMF solution, adding 150-170 mL of acetone into the DMF solution to obtain white powder slurry, performing suction filtration on the white powder slurry to remove filtrate and separate to obtain a product, placing the product in a vacuum drying oven with the set temperature of 80-90 ℃, and drying for 4-5 hours to obtain white powder; adding 10-15 parts by weight of methyl allyl polyoxyethylene ether, 5-7 parts by weight of polyacrylamide and 80-90 parts by weight of distilled water into a stirrer, heating to 50-55 ℃, adding 20-30 parts by weight of lignin powder, 5-10 parts by weight of 20% ammonium persulfate solution and 10-15 parts by weight of 30% sodium sulfite solution into the stirrer, carrying out heat preservation reaction for 3-4 h, cooling to room temperature, adding 70-80 parts by weight of ordinary portland cement, 20-25 parts by weight of fly ash, 10-15 parts by weight of magnesia and 20-25 parts by weight of white powder, and stirring and mixing at a rotating speed of 80-85 r/min to obtain the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
Example 1
Putting 200g of straw residues and 400mL of 45 mass percent sodium hydroxide solution into a water bath reaction kettle with a stirrer, heating in a water bath to 90 ℃, starting the stirrer, and stirring for 3 hours until the straw residues are completely dissolved to obtain lignin alkali liquor; neutralizing a lignin alkali liquor to be neutral by using glacial acetic acid with the mass fraction of 95% to obtain a lignin suspension, placing the lignin suspension in a high-speed centrifuge, centrifuging at a high speed of 3500r/min for 12min, removing a supernatant, separating to obtain a lower-layer precipitate, washing the precipitate for 2 times by using water, placing in an oven with the set temperature of 70 ℃, and drying for 4h to obtain lignin powder; adding 70g of beta-cyclodextrin and 100mL of 90% sodium hydroxide solution by mass into a beaker, stirring for 10min at room temperature, then adding 5g of epoxypropyl trimethyl ammonium chloride, placing the beaker into a water bath kettle, heating to 50 ℃, keeping the temperature for reaction for 3h, and filtering to remove filtrate to obtain a solid crude product; dissolving the solid crude product with 200mL of hot water at the temperature of 60 ℃, adjusting the pH to 6 with 10% of dilute hydrochloric acid by mass fraction to obtain a neutralized solution, placing the neutralized solution in a vacuum drying oven at the set temperature of 80 ℃, drying for 3h, and then placing in a mortar for grinding for 3h to obtain dry powder; dissolving 50g of dry powder by using 200mL of DMF to obtain a DMF solution, adding 150mL of acetone into the DMF solution to obtain white powder slurry, carrying out suction filtration on the white powder slurry to remove filtrate and separate to obtain a product, placing the product in a vacuum drying oven with the set temperature of 80 ℃, and drying for 4 hours to obtain white powder; adding 10 parts by weight of methyl allyl polyoxyethylene ether, 5 parts by weight of polyacrylamide and 80 parts by weight of distilled water into a stirrer, heating to 50 ℃, adding 20 parts by weight of lignin powder, 5 parts by weight of ammonium persulfate solution with the mass fraction of 20% and 10 parts by weight of sodium sulfite solution with the mass fraction of 30% into the stirrer, carrying out heat preservation reaction for 3 hours, cooling to room temperature, adding 70 parts by weight of ordinary portland cement, 20 parts by weight of fly ash, 10 parts by weight of magnesia and 20 parts by weight of white powder, and stirring and mixing at the rotating speed of 80r/min to obtain the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
Example 2
Putting 215g of straw residues and 425mL of 45 mass percent sodium hydroxide solution into a water bath reaction kettle with a stirrer, heating in a water bath to 93 ℃, starting the stirrer, and stirring for 4 hours until the straw residues are completely dissolved to obtain lignin alkali liquor; neutralizing a lignin alkali liquor to be neutral by using glacial acetic acid with the mass fraction of 95% to obtain a lignin suspension, placing the lignin suspension in a high-speed centrifuge, centrifuging at a high speed of 3600r/min for 14min, removing a supernatant, separating to obtain a lower-layer precipitate, washing the precipitate with water for 2 times, placing in an oven with the set temperature of 75 ℃, and drying for 4.5h to obtain lignin powder; adding 73g of beta-cyclodextrin and 115mL of 90% sodium hydroxide solution in mass fraction into a beaker, stirring for 13min at room temperature, adding 7g of epoxypropyltrimethylammonium chloride, placing the beaker into a water bath kettle, heating to 53 ℃, keeping the temperature for reaction for 3.5h, and filtering to remove filtrate to obtain a solid crude product; dissolving the solid crude product with 225mL of hot water at 63 ℃, adjusting the pH to 6.5 by using 10% of dilute hydrochloric acid by mass fraction to obtain a neutralized liquid, placing the neutralized liquid in a vacuum drying oven at 85 ℃, drying for 3.5h, and then placing in a mortar for grinding for 3.5h to obtain dry powder; dissolving 53g of dry powder by 210mL of DMF to obtain a DMF solution, adding 160mL of acetone into the DMF solution to obtain white powder slurry, carrying out suction filtration on the white powder slurry to remove filtrate and separate to obtain a product, placing the product in a vacuum drying oven with the set temperature of 85 ℃, and drying for 4.5 hours to obtain white powder; adding 13 parts by weight of methyl allyl polyoxyethylene ether, 6 parts by weight of polyacrylamide and 85 parts by weight of distilled water into a stirrer, heating to 53 ℃, adding 25 parts by weight of lignin powder, 7 parts by weight of ammonium persulfate solution with the mass fraction of 20% and 13 parts by weight of sodium sulfite solution with the mass fraction of 30% into the stirrer, carrying out heat preservation reaction for 3.5 hours, cooling to room temperature, adding 75 parts by weight of ordinary portland cement, 23 parts by weight of fly ash, 13 parts by weight of magnesia and 23 parts by weight of white powder, and stirring and mixing at the rotating speed of 83r/min to obtain the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
Example 3
230g of straw residues and 450mL of 45% sodium hydroxide solution by mass are put into a water bath reaction kettle with a stirrer, the water bath is heated to 95 ℃, the stirrer is started, and stirring is carried out for 5 hours until the straw residues are completely dissolved, so as to obtain lignin alkali liquor; neutralizing a lignin alkali liquor to be neutral by using glacial acetic acid with the mass fraction of 95% to obtain a lignin suspension, placing the lignin suspension in a high-speed centrifuge, centrifuging at a high speed for 15min at the rotating speed of 3700r/min, removing the supernatant, separating to obtain a lower-layer precipitate, washing the precipitate for 3 times by using water, placing in an oven with the set temperature of 80 ℃, and drying for 5 hours to obtain lignin powder; adding 75g of beta-cyclodextrin and 130mL of 90% sodium hydroxide solution by mass into a beaker, stirring for 15min at room temperature, adding 10g of epoxypropyl trimethyl ammonium chloride, placing the beaker into a water bath kettle, heating to 55 ℃, keeping the temperature for reaction for 4h, and filtering to remove filtrate to obtain a solid crude product; dissolving the solid crude product with 250mL of hot water at 65 ℃, adjusting the pH to 7 with 10% of dilute hydrochloric acid by mass fraction to obtain a neutralized liquid, placing the neutralized liquid in a vacuum drying oven at 90 ℃, drying for 4h, and then placing in a mortar for grinding for 4h to obtain dry powder; dissolving 55g of dry powder by 220mL of DMF to obtain a DMF solution, adding 170mL of acetone into the DMF solution to obtain white powder slurry, carrying out suction filtration on the white powder slurry to remove filtrate and separate to obtain a product, placing the product in a vacuum drying oven with a set temperature of 90 ℃, and drying for 5 hours to obtain white powder; adding 15 parts by weight of methyl allyl polyoxyethylene ether, 7 parts by weight of polyacrylamide and 90 parts by weight of distilled water into a stirrer, heating to 55 ℃, adding 30 parts by weight of lignin powder, 10 parts by weight of ammonium persulfate solution with the mass fraction of 20% and 15 parts by weight of sodium sulfite solution with the mass fraction of 30% into the stirrer, carrying out heat preservation reaction for 4 hours, cooling to room temperature, adding 80 parts by weight of ordinary portland cement, 25 parts by weight of fly ash, 15 parts by weight of magnesia and 25 parts by weight of white powder, and stirring and mixing at the rotating speed of 85r/min to obtain the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
Comparative example
The inorganic reinforcing steel bar anchoring adhesive produced by a certain company in Chongqing is used as a comparative example to detect the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive prepared by the invention and the inorganic reinforcing steel bar anchoring adhesive in the comparative example, and the detection results are shown in Table 1:
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Comparative example |
| Viscosity (cps) | 2752 | 2768 | 2773 | 2010 |
| Volume shrinkage (%) | 1.3 | 1.0 | 0.7 | 5.6 |
| Maximum drawing force (kN) | 196 | 201 | 213 | 145 |
According to the data in the table 1, the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive prepared by the invention has small volume shrinkage rate and strong bonding force between the anchoring adhesive and reinforcing steel bars, and is obviously superior to a comparative product. Therefore, the method has wide application prospect.
Claims (7)
1. A preparation method of a high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive is characterized by comprising the following specific preparation steps:
(1) putting 200-230 g of straw residues and 400-450 mL of sodium hydroxide solution into a water bath reaction kettle with a stirrer, heating in a water bath, starting the stirrer to stir until the straw residues are completely dissolved to obtain lignin alkali liquor;
(2) neutralizing a lignin alkali liquor to be neutral by using glacial acetic acid to obtain a lignin suspension, placing the lignin suspension in a high-speed centrifuge for high-speed centrifugation, removing supernatant, separating to obtain lower-layer precipitate, washing the precipitate with water for 2-3 times, placing in an oven, and drying to obtain lignin powder;
(3) adding 70-75 g of beta-cyclodextrin and 100-130 mL of sodium hydroxide solution into a beaker, stirring at room temperature, adding 5-10 g of epoxypropyl trimethyl ammonium chloride, placing the beaker in a water bath kettle, heating, carrying out heat preservation reaction, and filtering to remove filtrate to obtain a solid crude product;
(4) dissolving the solid crude product with 200-250 mL of hot water, adjusting the pH value with dilute hydrochloric acid to obtain a neutralized solution, placing the neutralized solution in a vacuum drying oven, drying, and then placing in a mortar for grinding to obtain dry powder;
(5) dissolving 50-55 g of dry powder by using 200-220 mL of DMF (dimethyl formamide) solution to obtain a DMF solution, adding 150-170 mL of acetone into the DMF solution to obtain white powder slurry, performing suction filtration on the white powder slurry to remove filtrate and separate to obtain a product, placing the product in a vacuum drying oven, and drying to obtain white powder;
(6) adding 10-15 parts by weight of methyl allyl polyoxyethylene ether, 5-7 parts by weight of polyacrylamide and 80-90 parts by weight of distilled water into a stirrer, heating to raise the temperature, adding 20-30 parts by weight of lignin powder, 5-10 parts by weight of ammonium persulfate solution and 10-15 parts by weight of sodium sulfite solution into the stirrer, carrying out heat preservation reaction, cooling to room temperature, adding 70-80 parts by weight of ordinary portland cement, 20-25 parts by weight of fly ash, 10-15 parts by weight of magnesia and 20-25 parts by weight of white powder, and stirring and mixing to obtain the high-viscosity low-shrinkage inorganic reinforcing steel bar anchoring adhesive.
2. The preparation method of the high-viscosity low-shrinkage inorganic reinforcing steel bar anchor adhesive according to claim 1, which is characterized by comprising the following steps of: the mass fraction of the sodium hydroxide solution in the step (1) is 45%, the temperature is 90-95 ℃ after water bath heating, and the stirring time is 3-5 h.
3. The preparation method of the high-viscosity low-shrinkage inorganic reinforcing steel bar anchor adhesive according to claim 1, which is characterized by comprising the following steps of: the mass fraction of the glacial acetic acid in the step (2) is 95%, the rotating speed of a high-speed centrifuge is 3500-3700 r/min, the high-speed centrifugation processing time is 12-15 min, the set temperature of an oven is 70-80 ℃, and the drying time is 4-5 h.
4. The preparation method of the high-viscosity low-shrinkage inorganic reinforcing steel bar anchor adhesive according to claim 1, which is characterized by comprising the following steps of: and (3) the mass fraction of the sodium hydroxide solution in the step (3) is 90%, the stirring time is 10-15 min, the temperature after heating and temperature rise is 50-55 ℃, and the heat preservation reaction time is 3-4 h.
5. The preparation method of the high-viscosity low-shrinkage inorganic reinforcing steel bar anchor adhesive according to claim 1, which is characterized by comprising the following steps of: the temperature of the hot water in the step (4) is 60-65 ℃, the mass fraction of the dilute hydrochloric acid is 10%, the pH value of the dilute hydrochloric acid is adjusted to 6-7, the set temperature of the vacuum drying oven is 80-90 ℃, the drying time is 3-4 h, and the grinding time in a mortar is 3-4 h.
6. The preparation method of the high-viscosity low-shrinkage inorganic reinforcing steel bar anchor adhesive according to claim 1, which is characterized by comprising the following steps of: and (5) setting the temperature of the vacuum drying oven to be 80-90 ℃, and drying for 4-5 hours.
7. The preparation method of the high-viscosity low-shrinkage inorganic reinforcing steel bar anchor adhesive according to claim 1, which is characterized by comprising the following steps of: and (3) after heating and temperature rising, the temperature is 50-55 ℃, the mass fraction of the ammonium persulfate solution is 20%, the mass fraction of the sodium sulfite solution is 30%, the reaction time is 3-4 h, and the stirring speed is 80-85 r/min.
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| CN108949071A (en) * | 2018-07-11 | 2018-12-07 | 翟琳 | A kind of preparation method of low viscous lower shrinkage impregnant |
| CN110028267A (en) * | 2019-03-27 | 2019-07-19 | 广州市浩恒建材科技有限公司 | A kind of preparation method of strong concrete polycarboxylate water-reducer |
| CN110372252A (en) * | 2019-06-12 | 2019-10-25 | 莫介勇 | A kind of preparation method of high degree of dispersion cladded type cement expansive material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE463673B (en) * | 1987-07-16 | 1991-01-07 | Cementa Ab | Bolt cement for securing bolts in boreholes in rock and concrete and anchoring prefabricated concrete elements, method for producing the bolt cement, and the use thereof |
| CN1332215A (en) * | 2001-08-10 | 2002-01-23 | 武汉大学 | Inorganic steel bar anchoring glue for concrete and its production process |
| CN101759856A (en) * | 2009-10-21 | 2010-06-30 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing sodium lignin sulfonate water reducer |
| CN104987029A (en) * | 2015-07-27 | 2015-10-21 | 重庆建工市政交通工程有限责任公司 | Inorganic post-anchoring grouting slurry |
-
2017
- 2017-12-01 CN CN201711246563.9A patent/CN108046690B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE463673B (en) * | 1987-07-16 | 1991-01-07 | Cementa Ab | Bolt cement for securing bolts in boreholes in rock and concrete and anchoring prefabricated concrete elements, method for producing the bolt cement, and the use thereof |
| CN1332215A (en) * | 2001-08-10 | 2002-01-23 | 武汉大学 | Inorganic steel bar anchoring glue for concrete and its production process |
| CN101759856A (en) * | 2009-10-21 | 2010-06-30 | 安徽丰原发酵技术工程研究有限公司 | Method for preparing sodium lignin sulfonate water reducer |
| CN104987029A (en) * | 2015-07-27 | 2015-10-21 | 重庆建工市政交通工程有限责任公司 | Inorganic post-anchoring grouting slurry |
Non-Patent Citations (1)
| Title |
|---|
| 羧甲基-β-环糊精减水剂的制备与性能;吕生华等;《材料导报》;材料导报;20120131;第132-135页 * |
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