CN108046690A - A kind of preparation method of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage - Google Patents

A kind of preparation method of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage Download PDF

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CN108046690A
CN108046690A CN201711246563.9A CN201711246563A CN108046690A CN 108046690 A CN108046690 A CN 108046690A CN 201711246563 A CN201711246563 A CN 201711246563A CN 108046690 A CN108046690 A CN 108046690A
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parts
steel bar
lignin
anchoring adhesive
bar anchoring
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CN108046690B (en
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高俊
何少雄
张建初
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Jiangsu Heyue New Material Technology Co., Ltd
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高俊
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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
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02Compositions 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
    • C04B28/04Portland cements
    • 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
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16Sulfur-containing compounds
    • C04B24/18Lignin sulfonic acid or derivatives thereof, e.g. sulfite lye
    • 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
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/38Polysaccharides or derivatives thereof
    • C04B24/383Cellulose or derivatives thereof
    • 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
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00637Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention relates to the reinforcement material preparing technical fields of building structure, and in particular to a kind of preparation method of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage.The present invention is using stalk as raw material, lignin lye is obtained by heating soda boiling, after lignin lye is neutralized with acetic acid, through high speed centrifugation, washing, it is dried to obtain lignin powder, homemade solid crude product is obtained into white powder by processing, dilution slurries are mixed into lignin powder and quartz sand, inorganic steel bar anchoring adhesive is made in flyash etc., quaternary ammonium cation cyclodextrin in the present invention can in water in colloidal form coat portland cement in anchor adhesive, cause portland cement particle in anchor adhesive mutually exclusive, improve the cohesive force between inorganic steel bar anchoring adhesive and reinforcing bar, add in a certain amount of lignin, shrinkage when inorganic steel bar anchoring adhesive quickly solidifies can be reduced, so as to enhance the cohesive force between inorganic steel bar anchoring adhesive and reinforcing bar, it has a extensive future.

Description

A kind of preparation method of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage
Technical field
The present invention relates to the reinforcement material preparing technical fields of building structure, and in particular to a kind of high viscous lower shrinkage is inorganic The preparation method of steel bar anchoring adhesive.
Background technology
Anchor adhesive is commonly called as anchoring adhesive, is mainly used to enhance the connection of concrete and rebar in building trade.Reinforced concrete Soil structure occupies extremely important status and considerable quantity in being built in China, with economic construction of China and the industrial structure Development, in recent years anchor adhesive obtained it is rapid development with being widely applied.
Common Bar Anchorage material is divided to organic and inorganic two major class.Organic anchoring material generally use epoxy based structures Glue, though intensity is high, poor water resistance, in wet condition adhesion strength it is low, ultraviolet light irradiation in the environment of be easy to aging, with The linear expansion coefficient difference of concrete is too big, the composition in yielding stripping, raw material mostly containing toxic or micro- toxicity, easily to people Body damages, and pollutes the environment.
At present, inorganic anchor adhesive in the market is mainly by portland-type cement or aluminium sulfate class cementitious composite various functions Additive, admixture and inorganic filler composition have the characteristics that solidifying, fast hard, fire resisting, shear strength be not high, afraid of water soon, while can It is constructed with cold operation and environmentally safe.It is mainly used for the underground engineerings anchor such as railway, tunnel, earthquake-resistant building, metallurgical mine Bar carries out leading the anchoring of nail in the rapid construction of supporting country rock and concrete structure reinforcement engineering, and can meet reinforcement welding It is required that.But it is inorganic anchoring adhesive there is also defect, such as:Bond strength is not high enough, and the inorganic anchor adhesive in part can table in the later stage Reveal certain shrinkage, the cohesive force of adhesive and concrete or steel is weak, causes adhesive bonds under constraint drawing condition The adhesion strength of reinforcing bar and base material concrete is unstable.Inorganic adhesive is limited to a certain extent in concrete structure reinforcement work Popularization and application in journey.
Therefore, developing a kind of inorganic steel bar anchoring adhesive that can solve above-mentioned performance issue is highly desirable.
The content of the invention
Present invention mainly solves the technical issues of, for inorganic steel bar anchoring adhesive, the phase can shrink and cause inorganic-steel after solidification The defects of cohesive force between muscle anchor adhesive and reinforcing bar dies down provides a kind of preparation of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage Method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage, it is characterised in that specifically preparation process is:
(1)200~230g stalks slag, 400~450mL sodium hydroxide solutions are put into the water-bath kettle with blender, Heating water bath heats up, and starts blender stirring, until stalk slag all dissolves, obtains lignin lye;
(2)Lignin lye is neutralized to neutrality with glacial acetic acid, obtains lignin suspension, lignin suspension is placed at a high speed Centrifuge high speed centrifuges, and removes supernatant liquor, and isolated lower sediment after precipitation 2~3 times is washed with water, is placed in baking oven In, it is dry, obtain lignin powder;
(3)70~75g beta-cyclodextrins and 100~130mL sodium hydroxide solutions are added in into beaker, after stirring at room temperature, then is added Enter 5~10g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath, heat temperature raising, insulation reaction, filtering removal filter Liquid obtains solid crude product;
(4)By solid crude product with 200~250mL hot water dissolvings, pH is adjusted with dilute hydrochloric acid, neutralizer is obtained, neutralizer is put In vacuum drying chamber, after dry, it be placed in mortar and grind, obtain dried powder;
(5)50~55g dried powders, 200~220mLDMF is dissolved, obtains DMF lysates, 150 are added in DMF lysates ~170mL acetone, obtains white slurry, and white slurry is filtered the removal isolated product of filtrate, product is placed in vacuum and is done It is dry in dry case, obtain white powder;
(6)It counts in parts by weight, 10~15 parts of methyl allyl polyoxyethylene ethers, 5~7 parts of polyacrylamides is added in into mixer Amine, 80~90 parts of distilled water, heat temperature raising, then 20~30 parts of lignin powder, 5~10 parts of ammonium persulfates are added in into mixer Solution, 10~15 parts of sodium sulfite solutions, insulation reaction add in 70~80 parts of Portland cements, 20 after being cooled to room temperature ~25 parts of flyash, 10~15 parts of magnesia, 20~25 parts of white powders are stirred, and obtain the inorganic Bar Anchorage of high viscous lower shrinkage Glue.
Step(1)The mass fraction of the sodium hydroxide solution is 45%, and temperature is 90~95 after heating water bath heating DEG C, mixing time is 3~5h.
Step(2)The mass fraction of the glacial acetic acid is 95%, and supercentrifuge rotating speed is 3500~3700r/min, high The fast centrifugal treating time is 12~15min, and baking oven design temperature is 70~80 DEG C, and drying time is 4~5h.
Step(3)The mass fraction of the sodium hydroxide solution be 90%, mixing time be 10~15min, heat temperature raising Temperature is 50~55 DEG C afterwards, and the insulation reaction time is 3~4h.
Step(4)The hot water temperature is 60~65 DEG C, and the mass fraction of dilute hydrochloric acid is 10%, and it is 6 that dilute hydrochloric acid, which adjusts pH, ~7, the design temperature of vacuum drying chamber is 80~90 DEG C, and drying time is 3~4h, and milling time is 3~4h in mortar.
Step(5)The design temperature of the vacuum drying chamber is 80~90 DEG C, and drying time is 4~5h.
Step(6)Temperature is 50~55 DEG C after the heat temperature raising, and the mass fraction of ammonium persulfate solution is 20%, sub- The mass fraction of metabisulfite solution is 30%, 3~4h of insulation reaction time, and speed of agitator is 80~85r/min.
The beneficial effects of the invention are as follows:
(1)The present invention obtains lignin lye using discarded stalk as raw material, by heating soda boiling, by lignin lye acetic acid After neutralization, through high speed centrifugation, wash, be dried to obtain lignin powder, epoxy is added in after beta-cyclodextrin is alkalized Solid crude product is obtained by filtration after ammonium chloride heating reaction, by solid crude product with hot water dissolving, by neutralizing, grinding, tying again White powder is obtained after crystalline substance purification, methyl allyl polyoxyethylene ether, polyacrylamide and distilled water are prepared, obtained dilute Slurries are released, then mix the inorganic major ingredient such as lignin powder and quartz sand, flyash, obtain inorganic steel bar anchoring adhesive, the present invention In white powder be purification after quaternary ammonium cation cyclodextrin, a small amount of quaternary ammonium cation cyclodextrin can be in water with glue Body form coats portland cement in anchor adhesive, and quaternary ammonium cation cyclodextrin is to the metal silicate surface in concrete Cation exclusion, after anchor adhesive quickly solidifies cohesive reinforcing bar, solidification later stage quaternary ammonium cation cyclodextrin is penetrated into anchor adhesive, is led It causes portland cement particle in anchor adhesive mutually exclusive, so that the shrinkage of anchor adhesive is reduced, improves inorganic Bar Anchorage Cohesive force between glue and reinforcing bar;
(2)Using the lignin recycled in stalk slag as the modified material of inorganic steel bar anchoring adhesive, lignin has the present invention in itself There is larger space structure, larger steric hindrance can be generated in inorganic steel bar anchoring adhesive, be conducive to improve inorganic reinforcing bar anchor The dispersion performance of solid glue, sodium sulfite and the lignin of addition occur sulfonating reaction, sulfonic acid group are introduced in lignin molecule, The hydrophilicity of inorganic steel bar anchoring adhesive can be improved, the high degree of dispersion of steel bar anchoring adhesive can be kept before solidification, is made inorganic Each region of steel bar anchoring adhesive keeps uniform density, reduces the shrinkage in solidification later stage, additionally incorporates a certain amount of lignin, can Increase the average molecular weight of inorganic steel bar anchoring adhesive, improve settled density of the anchor adhesive when rebar surface bonds, reduce inorganic Shrinkage when steel bar anchoring adhesive quickly solidifies, so as to enhance the cohesive force between inorganic steel bar anchoring adhesive and reinforcing bar, before Scape is wide.
Specific embodiment
200~230g stalks slag, the sodium hydroxide solution that 400~450mL mass fractions are 45% are put into blender Water-bath kettle in, heating water bath is warming up to 90~95 DEG C, starts blender, stirs 3~5h, until stalk slag is all molten Solution, obtains lignin lye;Lignin lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, lignin is obtained and hangs Lignin suspension is placed in supercentrifuge by supernatant liquid, with the rotating speed of 3500~3700r/min, high speed centrifugation 12~ 15min, removes supernatant liquor, and isolated lower sediment after precipitation 2~3 times is washed with water, is placed in design temperature as 70~80 DEG C baking oven in, dry 4~5h obtains lignin powder;70~75g beta-cyclodextrins and 100~130mL matter are added in into beaker The sodium hydroxide solution that fraction is 90% is measured, after stirring 10~15min at room temperature, adds 5~10g epoxy chlorine Change ammonium, beaker is placed in water-bath, be heated to 50~55 DEG C, 3~4h of insulation reaction, filtering removal filtrate obtains solid Crude product;With 200~250mL temperature it is 60~65 DEG C of hot water dissolving by solid crude product, with dilute salt that mass fraction is 10% Acid for adjusting pH obtains neutralizer, neutralizer is placed in the vacuum drying chamber that design temperature is 80~90 DEG C, dry 3 to 6~7 After~4h, 3~4h of grinding in mortar is placed in, obtains dried powder;50~55g dried powders, 200~220mLDMF is dissolved, DMF lysates are obtained, 150~170mL acetone is added in DMF lysates, obtains white slurry, white slurry is filtered into removal filter Product is placed in the vacuum drying chamber that design temperature is 80~90 DEG C by the isolated product of liquid, and dry 4~5h obtains white Powder;It counts in parts by weight, 10~15 parts of methyl allyl polyoxyethylene ethers, 5~7 parts of polyacrylamides is added in into mixer Amine, 80~90 parts of distilled water, after being heated to 50~55 DEG C, then into mixer add in 20~30 parts of lignin powder, 5~ The ammonium persulfate solution that 10 parts of mass fractions are 20%, the sodium sulfite solution that 10~15 parts of mass fractions are 30%, insulation reaction 3 ~4h, be cooled to after room temperature add in 70~80 parts of Portland cements, 20~25 parts of flyash, 10~15 parts of magnesia, 20~ 25 parts of white powders are stirred with the rotating speed of 80~85r/min, obtain the inorganic steel bar anchoring adhesive of high viscous lower shrinkage.
Example 1
200g stalks slag, the sodium hydroxide solution that 400mL mass fractions are 45% are put into the water-bath kettle with blender In, heating water bath is warming up to 90 DEG C, starts blender, stirs 3h, until stalk slag all dissolves, obtains lignin lye;It will Lignin lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension, lignin suspension is put In supercentrifuge, with the rotating speed of 3500r/min, high speed centrifugation 12min removes supernatant liquor, isolated lower sediment, It is washed with water after precipitating 2 times, is placed in the baking oven that design temperature is 70 DEG C, dry 4h obtains lignin powder;Add into beaker Enter 70g beta-cyclodextrins and 100mL mass fractions for 90% sodium hydroxide solution, after stirring 10min at room temperature, add 5g rings Oxygen propyl group trimethyl ammonium chloride, beaker is placed in water-bath, is heated to 50 DEG C, insulation reaction 3h, filtering removal filtrate Obtain solid crude product;With 200mL temperature it is 60 DEG C of hot water dissolving by solid crude product, with dilute salt that mass fraction is 10% Acid for adjusting pH obtains neutralizer, neutralizer is placed in the vacuum drying chamber that design temperature is 80 DEG C, after dry 3h, is placed in 6 3h is ground in mortar, obtains dried powder;50g dried powders with 200mLDMF are dissolved, obtain DMF lysates, are dissolved to DMF Liquid adds in 150mL acetone, obtains white slurry, and white slurry is filtered the removal isolated product of filtrate, product is placed in and is set Constant temperature degree is in 80 DEG C of vacuum drying chamber, and dry 4h obtains white powder;It counts in parts by weight, 10 is added in into mixer Part methyl allyl polyoxyethylene ether, 5 parts of polyacrylamides, 80 parts of distilled water, after being heated to 50 DEG C, then into mixer Add in 20 parts of lignin powder, the ammonium persulfate solution that 5 parts of mass fractions are 20%, the sodium sulfite that 10 parts of mass fractions are 30% Solution, insulation reaction 3h, be cooled to after room temperature add in 70 parts of Portland cements, 20 parts of flyash, 10 parts of magnesia, 20 parts it is white Color powder is stirred with the rotating speed of 80r/min, obtains the inorganic steel bar anchoring adhesive of high viscous lower shrinkage.
Example 2
215g stalks slag, the sodium hydroxide solution that 425mL mass fractions are 45% are put into the water-bath kettle with blender In, heating water bath is warming up to 93 DEG C, starts blender, stirs 4h, until stalk slag all dissolves, obtains lignin lye;It will Lignin lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension, lignin suspension is put In supercentrifuge, with the rotating speed of 3600r/min, high speed centrifugation 14min removes supernatant liquor, isolated lower sediment, It is washed with water after precipitating 2 times, is placed in the baking oven that design temperature is 75 DEG C, dry 4.5h obtains lignin powder;Into beaker 73g beta-cyclodextrins and 115mL mass fractions are added in as 90% sodium hydroxide solution, after stirring 13min at room temperature, adds 7g Beaker is placed in water-bath by epoxypropyltrimethylchloride chloride, is heated to 53 DEG C, insulation reaction 3.5h, filtering removal Filtrate obtains solid crude product;With 225mL temperature it is 63 DEG C of hot water dissolving by solid crude product, is 10% with mass fraction Dilute hydrochloric acid adjusts pH to 6.5, obtains neutralizer, neutralizer is placed in the vacuum drying chamber that design temperature is 85 DEG C, dry It after 3.5h, is placed in mortar and grinds 3.5h, obtain dried powder;53g dried powders with 210mLDMF are dissolved, it is molten to obtain DMF Liquid is solved, 160mL acetone is added in DMF lysates, obtains white slurry, white slurry is filtered into the removal isolated production of filtrate Product is placed in the vacuum drying chamber that design temperature is 85 DEG C by object, and dry 4.5h obtains white powder;It counts in parts by weight, 13 parts of methyl allyl polyoxyethylene ethers, 6 parts of polyacrylamides, 85 parts of distilled water are added in into mixer, are heated to 53 After DEG C, then add in 25 parts of lignin powder into mixer, the ammonium persulfate solution that 7 parts of mass fractions are 20%, 13 parts of quality point Number is 30% sodium sulfite solution, and insulation reaction 3.5h adds in 75 parts of Portland cements, 23 parts of powder after being cooled to room temperature Coal ash, 13 parts of magnesia, 23 parts of white powders are stirred with the rotating speed of 83r/min, obtain the inorganic Bar Anchorage of high viscous lower shrinkage Glue.
Example 3
230g stalks slag, the sodium hydroxide solution that 450mL mass fractions are 45% are put into the water-bath kettle with blender In, heating water bath is warming up to 95 DEG C, starts blender, stirs 5h, until stalk slag all dissolves, obtains lignin lye;It will Lignin lye is neutralized to neutrality with the glacial acetic acid that mass fraction is 95%, obtains lignin suspension, lignin suspension is put In supercentrifuge, with the rotating speed of 3700r/min, high speed centrifugation 15min removes supernatant liquor, isolated lower sediment, It is washed with water after precipitating 3 times, is placed in the baking oven that design temperature is 80 DEG C, dry 5h obtains lignin powder;Add into beaker Enter 75g beta-cyclodextrins and 130mL mass fractions for 90% sodium hydroxide solution, after stirring 15min at room temperature, add 10g rings Oxygen propyl group trimethyl ammonium chloride, beaker is placed in water-bath, is heated to 55 DEG C, insulation reaction 4h, filtering removal filtrate Obtain solid crude product;With 250mL temperature it is 65 DEG C of hot water dissolving by solid crude product, with dilute salt that mass fraction is 10% Acid for adjusting pH obtains neutralizer, neutralizer is placed in the vacuum drying chamber that design temperature is 90 DEG C, after dry 4h, is placed in 7 4h is ground in mortar, obtains dried powder;55g dried powders with 220mLDMF are dissolved, obtain DMF lysates, are dissolved to DMF Liquid adds in 170mL acetone, obtains white slurry, and white slurry is filtered the removal isolated product of filtrate, product is placed in and is set In fixed vacuum drying chamber at a temperature of 90 °C, dry 5h obtains white powder;It counts in parts by weight, 15 is added in into mixer Part methyl allyl polyoxyethylene ether, 7 parts of polyacrylamides, 90 parts of distilled water, after being heated to 55 DEG C, then into mixer Add in 30 parts of lignin powder, the ammonium persulfate solution that 10 parts of mass fractions are 20%, the sulfurous acid that 15 parts of mass fractions are 30% Sodium solution, insulation reaction 4h, be cooled to after room temperature add in 80 parts of Portland cements, 25 parts of flyash, 15 parts of magnesia, 25 parts White powder is stirred with the rotating speed of 85r/min, obtains the inorganic steel bar anchoring adhesive of high viscous lower shrinkage.
Comparative example
It is inorganic to high viscous lower shrinkage produced by the present invention as a comparison case with the inorganic steel bar anchoring adhesive of company of Chongqing City production Inorganic steel bar anchoring adhesive in steel bar anchoring adhesive and comparative example is detected, and testing result is as shown in table 1:
Table 1
Test event Example 1 Example 2 Example 3 Comparative example
Viscosity(cps) 2752 2768 2773 2010
Cubical contraction(%) 1.3 1.0 0.7 5.6
Draft(kN) 196 201 213 145
According to data in table 1, the inorganic steel bar anchoring adhesive of high viscous lower shrinkage produced by the present invention, cubical contraction is small, anchoring The cohesive force of glue and reinforcing bar is strong, hence it is evident that better than comparative example product.Therefore, there is wide prospect of the application.

Claims (7)

1. a kind of preparation method of the high viscous inorganic steel bar anchoring adhesive of lower shrinkage, it is characterised in that specifically preparation process is:
(1)200~230g stalks slag, 400~450mL sodium hydroxide solutions are put into the water-bath kettle with blender, Heating water bath heats up, and starts blender stirring, until stalk slag all dissolves, obtains lignin lye;
(2)Lignin lye is neutralized to neutrality with glacial acetic acid, obtains lignin suspension, lignin suspension is placed at a high speed Centrifuge high speed centrifuges, and removes supernatant liquor, and isolated lower sediment after precipitation 2~3 times is washed with water, is placed in baking oven In, it is dry, obtain lignin powder;
(3)70~75g beta-cyclodextrins and 100~130mL sodium hydroxide solutions are added in into beaker, after stirring at room temperature, then is added Enter 5~10g epoxypropyltrimethylchloride chlorides, beaker is placed in water-bath, heat temperature raising, insulation reaction, filtering removal filter Liquid obtains solid crude product;
(4)By solid crude product with 200~250mL hot water dissolvings, pH is adjusted with dilute hydrochloric acid, neutralizer is obtained, neutralizer is put In vacuum drying chamber, after dry, it be placed in mortar and grind, obtain dried powder;
(5)50~55g dried powders, 200~220mLDMF is dissolved, obtains DMF lysates, 150 are added in DMF lysates ~170mL acetone, obtains white slurry, and white slurry is filtered the removal isolated product of filtrate, product is placed in vacuum and is done It is dry in dry case, obtain white powder;
(6)It counts in parts by weight, 10~15 parts of methyl allyl polyoxyethylene ethers, 5~7 parts of polyacrylamides is added in into mixer Amine, 80~90 parts of distilled water, heat temperature raising, then 20~30 parts of lignin powder, 5~10 parts of ammonium persulfates are added in into mixer Solution, 10~15 parts of sodium sulfite solutions, insulation reaction add in 70~80 parts of Portland cements, 20 after being cooled to room temperature ~25 parts of flyash, 10~15 parts of magnesia, 20~25 parts of white powders are stirred, and obtain the inorganic Bar Anchorage of high viscous lower shrinkage Glue.
2. a kind of preparation method of high viscous inorganic steel bar anchoring adhesive of lower shrinkage according to claim 1, it is characterised in that:Step Suddenly(1)The mass fraction of the sodium hydroxide solution is 45%, and temperature is 90~95 DEG C after heating water bath heating, mixing time For 3~5h.
3. a kind of preparation method of high viscous inorganic steel bar anchoring adhesive of lower shrinkage according to claim 1, it is characterised in that:Step Suddenly(2)The mass fraction of the glacial acetic acid is 95%, and supercentrifuge rotating speed is 3500~3700r/min, and high speed centrifugation is handled Time is 12~15min, and baking oven design temperature is 70~80 DEG C, and drying time is 4~5h.
4. a kind of preparation method of high viscous inorganic steel bar anchoring adhesive of lower shrinkage according to claim 1, it is characterised in that:Step Suddenly(3)The mass fraction of the sodium hydroxide solution is 90%, and mixing time is 10~15min, and temperature is 50 after heat temperature raising ~55 DEG C, the insulation reaction time is 3~4h.
5. a kind of preparation method of high viscous inorganic steel bar anchoring adhesive of lower shrinkage according to claim 1, it is characterised in that:Step Suddenly(4)The hot water temperature is 60~65 DEG C, and the mass fraction of dilute hydrochloric acid is 10%, and it is 6~7 that dilute hydrochloric acid, which adjusts pH, and vacuum is done The design temperature of dry case is 80~90 DEG C, and drying time is 3~4h, and milling time is 3~4h in mortar.
6. a kind of preparation method of high viscous inorganic steel bar anchoring adhesive of lower shrinkage according to claim 1, it is characterised in that:Step Suddenly(5)The design temperature of the vacuum drying chamber is 80~90 DEG C, and drying time is 4~5h.
7. a kind of preparation method of high viscous inorganic steel bar anchoring adhesive of lower shrinkage according to claim 1, it is characterised in that:Step Suddenly(6)Temperature is 50~55 DEG C after the heat temperature raising, and the mass fraction of ammonium persulfate solution is 20%, sodium sulfite solution Mass fraction for 30%, 3~4h of insulation reaction time, speed of agitator is 80~85r/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
CN110467396A (en) * 2019-08-30 2019-11-19 李魁 A kind of preparation method of cracking resistance lower shrinkage cement mortar

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