CN101665336A - Preparation method of low-alkaline liquid accelerating agent - Google Patents
Preparation method of low-alkaline liquid accelerating agent Download PDFInfo
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- CN101665336A CN101665336A CN200910183568A CN200910183568A CN101665336A CN 101665336 A CN101665336 A CN 101665336A CN 200910183568 A CN200910183568 A CN 200910183568A CN 200910183568 A CN200910183568 A CN 200910183568A CN 101665336 A CN101665336 A CN 101665336A
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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
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
- C04B24/122—Hydroxy amines
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/14—Hardening accelerators
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a preparation method of low-alkaline liquid accelerating agent, comprising the following steps: 1) preparing sodium aluminate liquid; 2) modifying sodium aluminate liquid; 3)carrying out a reaction between the modified sodium aluminate and the aluminum sulfate; and 4) adding hydramine and hydroxycarboxylic acid and stirring evenly to prepare the finished product. The low-alkaline liquid accelerating agent prepared by the invention has low alkali content, namely, the sum of Na2O and K2O is less than 5%, low preparation cost, is suitable for cement such as ordinary Portland cement, moderate-heat cement, low-heat cement and other brands and types, is applicable to the sprayed concrete construction, can significantly improve initial strength and ensure later strength.
Description
Technical field
The present invention relates to a kind of preparation method of low-alkali liquid quick-setting agent, prepared low-alkali liquid quick-setting agent is applicable to the wet spraying concrete.
Background technology
Sprayed concrete has lot of superiority in underground construction and rock support, become extremely important and necessary measure in the modern underground works.Along with the development of wet-mix shotcrete technology, expanded the use range of sprayed concrete in underground works greatly.The most important effect of liquid accelerator for sprayed concrete is to accelerate condensing of concrete mix, improves early strength, can increase jetting thickness and shortening like this and spray the pitch time of one deck down.
Traditional shotcrete accelerator generally comprises materials such as alkali metal aluminate, carbonate, silicate.Because these materials all have strong basicity, in construction, often bring a lot of problems.Such as, the alkali metal aluminate accelerating chemicals often has very strong caustic corrosion, easily the workmen is damaged; Can cause bad influence to environment.Simultaneously because a large amount of uses of alkaline matter, late strength of concrete can exist 30% even bigger reduction.
In order to overcome the above problems, people have developed the liquid accelerator of some alkali-free metal ions.For example German construction research and technology limited liability company have developed a kind of " accelerating chemicals that is used for sprayed concrete " (Chinese patent application number be 200580025329.2), a kind of solution or fine suspension that it is made up of Tai-Ace S 150 and dissolved hydrogen aluminum oxide, hydroxycarboxylic acid and alcamines material.Switzerland MBT Holding AG discloses " a kind of concrete with the preparation of accelerating chemicals " (China Patent No. is 00816806.7), and it is to be dissolved in the water that contains amine by Tai-Ace S 150 and unformed aluminium hydroxide, and adds stablizer and defoamer makes.Above-mentioned alkali-free quick-coagulant has solved the alkali-aggregate reaction problem of sprayed concrete to a certain extent, and volume is very high during still owing to use, causes the sprayed concrete cost significantly to improve, and is unfavorable for applying.In addition, the same with alkaline accelerating chemicals, existing alkali-free quick-coagulant does not solve cement adaptability well.
Liquid accelerator join in the sprayed concrete mixture with cement in mineral hydration reaction fast takes place, cement is condensed at short notice, early strength increases rapidly.The action effect of accelerating chemicals and the mineral constituent in the cement and content have confidential relation, yet Cement Production is subjected to the influence of numerous factors such as starting material, production technique, mineral composition obvious difference.In China, can contain in the ordinary Portland cement and be not more than 20% nonactive adulterant, and adulterant is of a great variety, so the cement adaptability of liquid accelerator is very outstanding, influences its use in sprayed concrete.
Summary of the invention
The objective of the invention is to overcome existing alkaline accelerating chemicals and alkali-free quick-coagulant shortcoming separately, put forward the preparation method of the liquid accelerator for sprayed concrete of a kind of low alkalinity of generation.
The applicant thinks, the alkaline accelerating chemicals that with the aluminate is main component mainly be with cement in gypsum reaction fast takes place, eliminate it delayed coagulation of calcium aluminate in the cement made the cement rapid coagulation.And alkali-free quick-coagulant mainly be wherein Tai-Ace S 150 by with cement slurry in calcium hydroxide, calcium aluminate and gypsum be swift in response and generate ettringite and make the fast accelerating chemicals of cement.As seen these two kinds of accelerating chemicalss have very strong complementarity for the blood coagulation enhancing effect of cement, provide thinking for solving accelerating chemicals to cement adaptability.
Based on above-mentioned thinking, the applicant is this discovery after deliberation, the liquid accelerator that with the aluminate is main component mixes in the cement slurry simultaneously as being aided with part of sulfuric acid aluminium again, and its short effect of coagulating can significantly improve, and works particularly evident for the cement of aluminate accelerating chemicals bad adaptability.
Because liquid sodium aluminate and Tai-Ace S 150 are two kinds of antipodal materials of acid-basicity, use ordinary method to be difficult to be implemented in the solution and coexist.But, use for reference the correlation technique in other technologies field, under high shear conditions, the liquid sodium aluminate can be dissolved in the alum liquor and form stable solution, so just can be combined into a kind of uniform solution with being difficult to miscible material under sodium aluminate and these two kinds of normal conditions of Tai-Ace S 150.
The applicant also finds after deliberation, though the sodium aluminate of one-component can be dissolved in the alum liquor under shear conditions gradually, but its less stable, and can significantly improve the stability of the finished product through the sodium aluminate solution of persilicate, carbonate modification.
Above-mentioned high-shear agitation condition is the well-known technical qualification of a kind of chemical field, and available common mixing machine, homogenizer are realized.The basic definition of fluid shearing speed is velocity slope dv/dy, and its unit is the inverse (S of time
-1).
Based on above-mentioned research, the applicant proposes a kind of preparation method of low-alkaline liquid accelerating agent, and this method comprises the steps:
1) liquid sodium aluminate preparation: sodium hydroxide and aluminium hydroxide are prepared into the liquid sodium aluminate according to 1.1: 1.5 mol ratio, and wherein the content of aluminum oxide is 20～30wt%;
2) modification of liquid sodium aluminate: at first water glass, yellow soda ash are added and be mixed with properties-correcting agent in the entry, the content of this properties-correcting agent mesosilicic acid sodium is 15～45%, and carbonate content is 5～15%; Secondly, the liquid sodium aluminate that step 1) is made adds in the properties-correcting agent, and the mass ratio of sodium aluminate and properties-correcting agent is 6: 1～2.5: 1; The liquid aluminic acid is received in the modifying process, need add entry, the add-on of water be the liquid sodium aluminate weight 50%;
3) reaction of modification sodium aluminate and Tai-Ace S 150: with step 2) to be added drop-wise to alumina content be in 7.5～9% the alum liquor, to make stabilizing solution to the modified liquid sodium aluminate that makes; The mass ratio of modified liquid sodium aluminate and alum liquor is 1: 4～1: 8;
4) add hydramine and hydroxycarboxylic acid, stirring promptly makes finished product; The content of hydroxycarboxylic acid is that the content of 0.5～3wt%, hydramine is 0.5～5% in the finished product.
In the step 1), at first that sodium hydroxide is soluble in water, be heated to 80～130 ℃, add aluminium hydroxide then; Under said temperature, react and to obtain the liquid sodium aluminate in 2～6 hours.The optional conversion unit that carries reflux of reactor.Preferred 90～110 ℃ of temperature of reaction, preferred 3～5 hours of reaction times.
Step 2) preferred 5: 1～3.5: 1 of the mass ratio of sodium aluminate and properties-correcting agent in, the liquid sodium aluminate is being added in the process of properties-correcting agent, water adds when gel occurring, treats that gel dissolving back continuation adds remaining liquid aluminium acid sodium solution, makes the modified liquid sodium aluminate.Step 2) whole process need carries out being not less than under the 1000S-1 high-shear agitation condition, disperses to add supergrip, and the reaction times is 0.5～2 hour.
The mass ratio of modified liquid sodium aluminate and alum liquor is preferred 1: 5～1: 6 in the step 3); Adopt the high speed shear stirrer in the dropping process, be not less than 3000S
-1Carry out under the shear conditions, reunite with the aluminum hydroxide gel that prevents to form and lump; The dropping time is 30～90 minutes, preferred 40～60 minutes; Whole process should be carried out under 10～30 ℃ temperature; After being added dropwise to complete, solution temperature is slowly risen to 50～60 ℃, the heating-up time should greater than 30 minutes (why will control heat-up rate be for preventing that Tai-Ace S 150, sodium aluminate from reacting too violent); Be incubated 1～2 hour then, obtain brown xanchromatic clear solution.
Hydramine in the step 4) is selected from trolamine, diethanolamine or Monoethanolamine MEA BASF, preferred diethanolamine and trolamine, more preferably diethanolamine; Hydroxycarboxylic acid is selected from formic acid, lactic acid or oxyacetic acid.The addition sequence of hydramine and carboxylic acid there is no particular requirement, adds hydramine again after can earlier the carboxylic acid adding being stirred, and adds hydroxycarboxylic acid again after also can earlier the hydramine adding being stirred.
Adopt the application method of the low-alkaline liquid accelerating agent of the present invention's preparation to be: according to routine liquid accelerator is joined in the sprayed concrete mixture and prepare sprayed concrete, its usage quantity is 5～8% of a cement consumption.
The present invention has successfully made a kind of stable low-alkaline liquid accelerating agent with sodium aluminate, two kinds of materials of Tai-Ace S 150, this liquid accelerator has possessed Liquid Aluminate Accelerating Additive and Tai-Ace S 150 is the characteristic of the alkali-free quick-coagulant of main component, has better cement adaptability, and employed starting material are common chemical raw material among the present invention, help controlling cost.
The present invention has following positive effect:
1,, adopt the low-alkaline liquid accelerating agent of the present invention's preparation promptly can make cement initial set within 4 minutes, final set within 10 minutes at (5%～8%) under the lower volume according to the experiment condition of JC477-2005 " sprayed concrete accelerating chemicals ".
2, according to the test conditions of JC477-2005 " sprayed concrete accelerating chemicals ", the 1 day intensity that the low-alkaline liquid accelerating agent that adopts the present invention to prepare can make sand-cement slurry is more than 10Mpa, and the intensity storage rate was greater than 80% in 28 days.
3, the alkali content of the low-alkaline liquid accelerating agent of employing the present invention preparation can make various cement satisfy requirement time of coagulation less than 5%.
Embodiment
Following example has been described the process of low-alkaline liquid accelerating agent prepared according to the methods of the invention in more detail, and these examples provide in the mode of explanation, but these examples not delimit the scope of the invention.As not explanation in addition, umber is meant weight part.
One, the preparation of liquid sodium aluminate
The liquid sodium aluminate prepares embodiment 1
25 parts of solid sodium hydroxides are dissolved in 43 parts of water, under 80 ℃ condition, 32 parts of aluminium hydroxides are added wherein (mol ratio of sodium hydroxide and aluminium hydroxide is 1.4) then, reacted 6 hours, make Al
2O
3Content is 20% liquid sodium aluminate E-1..Reaction vessel is the there-necked flask of band thermometer and reflux.
The liquid sodium aluminate prepares embodiment 2
25 parts of solid sodium hydroxides are dissolved in 30 parts of water, under 100 ℃ condition, 45 parts of aluminium hydroxides are added wherein (mol ratio of sodium hydroxide and aluminium hydroxide is 1.1) then, reacted 4 hours, make Al
2O
3Content is 30% liquid sodium aluminate E-2..Reaction vessel is the there-necked flask of band thermometer and reflux
The liquid sodium aluminate prepares embodiment 3
25 parts of solid sodium hydroxides are dissolved in 33 parts of water, under 130 ℃ condition, 42 parts of aluminium hydroxides are added wherein (mol ratio of sodium hydroxide and aluminium hydroxide is 1.1) then, reacted 2 hours, make Al
2O
3Content is 27.5% liquid sodium aluminate E-2..Reaction vessel is the there-necked flask of band thermometer and reflux
Table 1: liquid sodium aluminate E1-E3
Two, liquid sodium aluminate modification
Press table 2 configuration sodium aluminate water glass mixing solutions
Table 2. water glass, sodium carbonate mixture
Liquid sodium aluminate modification embodiment 1
Stir (1000S in high-shear
-1) state 50 parts of liquid sodium aluminates (E1) are slowly joined in 20 parts of H1 solution.When gel occurring, add 25 parts of water, treat that gel dissolving back continuation adds remaining liquid aluminium acid sodium solution, continue 0.5 hour system of reaction, get modified liquid sodium aluminate G-1.
Liquid sodium aluminate modification embodiment 2
Stir (1500S in high-shear
-1) state 50 parts of liquid sodium aluminates (E2) are slowly joined in 12.5 parts of H2 solution.When gel occurring, add 25 parts of water, treat that gel dissolving back continuation adds remaining liquid aluminium acid sodium solution, continue reflection 1 hour, make modified liquid sodium aluminate G-2.
Liquid sodium aluminate modification embodiment 3
Stir (1000S in high-shear
-1) state 50 parts of liquid sodium aluminates (E3) are slowly joined in 8.5 parts of H3 solution.When gel appears in meeting, add 25 parts of water, treat that gel dissolving back continuation adds remaining liquid aluminium acid sodium solution, continue reaction 2 hours, make modified liquid sodium aluminate G-3.
Three, modification sodium aluminate and reacting aluminum sulfate
Reaction embodiment 1
With 100 parts of G-1, slowly be added drop-wise to 550 parts of alumina contents and be in 9% the alum liquor.Adopt high-shear to stir shape (3000S in the dropping process
-1) carry out under the attitude, with the aluminum hydroxide gel that prevents from the to form caking of reuniting.The dropping time is about 30 minutes, and whole process should be carried out under the temperature about 20 ℃; After being added dropwise to complete, solution temperature is slowly risen to 50 ℃, 30 minutes heating-up times of control; Be incubated 1 hour then, obtain brown xanchromatic clear solution L-1.
Reaction embodiment 2
With 100 parts of G-2, slowly be added drop-wise to 400 parts of alumina contents and be in 8.2% the alum liquor, adopt high-shear to stir shape (5000S in the dropping process
-1) carry out under the attitude, with the aluminum hydroxide gel that prevents from the to form caking of reuniting.The dropping time is about 60 minutes, and whole process should be carried out under the temperature about 10 ℃; After being added dropwise to complete, solution temperature is slowly risen to 55 ℃, 45 minutes heating-up times of control; Be incubated 1.5 hours then, obtain brown xanchromatic clear solution L-2.
Reaction embodiment 3
With 100 parts of G-3, slowly be added drop-wise to 800 parts of alumina contents and be in 9% the alum liquor, adopt high-shear to stir shape (3000S in the dropping process
-1) carry out under the attitude, with the aluminum hydroxide gel that prevents from the to form caking of reuniting.The dropping time is about 90 minutes, and whole process should be carried out under the temperature about 30 ℃; After being added dropwise to complete, solution temperature is slowly risen to 60 ℃, 60 minutes heating-up times of control; Be incubated 2 hours then, obtain brown xanchromatic clear solution L-3.
Four, the allotment of accelerating chemicals
Allotment embodiment 1
Join formic acid, diethanolamine among the prepared product L-1 of step (three) successively and stir, make and contain 0.5% formic acid, 1% trolamine in the final product, obtain low-alkaline liquid accelerating agent P-1.
Allotment embodiment 2
Join formic acid, diethanolamine among the prepared product L-2 of step (three) successively and stir, make and contain 1% formic acid, 3% diethanolamine in the final product, obtain low-alkaline liquid accelerating agent P-2.
Allotment embodiment 3
Join lactic acid, diethanolamine among the prepared product L-3 of step (three) successively and stir, make and contain 3% lactic acid, 5% trolamine in the final product, obtain low-alkaline liquid accelerating agent P-3.
Application example 1
Carry out cement paste time of coagulation and strength of cement mortar test according to the requirement of Chinese building material industry standard JC477-2005 " sprayed concrete accelerating chemicals ".Wherein the liquid accelerator consumption is according to the percentage calculation of cement weight.
Cement paste test time of coagulation
Lafarge PO.42.5 cement 400
Water 160
The strength of cement mortar test
Lafarge PO42.5 cement 900
Standard sand 1350
Water 450
Accelerating chemicals adds in the cement slurry according to 7% of cement weight, and above-mentioned water consumption has comprised water contained in the liquid accelerator simultaneously.In the strength test, except testing 1 day intensity and 28 days intensity, do not carried out strength trial, be mixed with mortar and its 28 days strength ratio in order to test to adding the blank mortar of any quick-hardening.Test-results such as table 1.
Table 1. accelerating chemicals effect
Liquid accelerator for sprayed concrete among the present invention can make satisfy presetting period less than 5 minute the time of coagulation of cement paste under 7% volume, and final setting time was less than 12 minutes requirement.Mortar strength was reached more than the 14Mpa, the 6Mpa in the Chinese building material industry standard at one day.
Application example 2
Example 3 prepared liquid accelerator for sprayed concrete are carried out time of coagulation and mortar strength experiment according to JC477-2005 " sprayed concrete accelerating chemicals " for dissimilar and cement brand, the sample that simultaneous test selects for use commercially available aluminate class liquid accelerator to select for use is P-2, and test-results is as follows:
The contrast of table 2. accelerating chemicals effect
Low-alkali liquid quick-setting agent provided by the invention can make dissimilar and cement brand satisfy the construction requirement of sprayed concrete, has good cement adaptability.
Claims (12)
1, a kind of preparation method of low-alkaline liquid accelerating agent is characterized in that comprising the steps:
1) liquid sodium aluminate preparation: sodium hydroxide and aluminium hydroxide are prepared into the liquid sodium aluminate according to 1.1: 1.5 mol ratio, and wherein the content of aluminum oxide is 20～30wt%;
2) modification of liquid sodium aluminate: at first water glass, yellow soda ash are added and be mixed with properties-correcting agent in the entry, the content of this properties-correcting agent mesosilicic acid sodium is 15～45%, and carbonate content is 5～15%; Secondly, the liquid sodium aluminate that step 1) is made adds in the properties-correcting agent, and the mass ratio of sodium aluminate and properties-correcting agent is 6: 1～2.5: 1; The liquid aluminic acid is received in the modifying process, need add entry, the add-on of water be the liquid sodium aluminate weight 50%;
3) reaction of modification sodium aluminate and Tai-Ace S 150: with step 2) to be added drop-wise to alumina content be in 7.5～9% the alum liquor, to make stabilizing solution to the modified liquid sodium aluminate that makes; The mass ratio of modified liquid sodium aluminate and alum liquor is 1: 4～1: 8;
4) add hydramine and hydroxycarboxylic acid, stirring promptly makes finished product; The content of hydroxycarboxylic acid is that the content of 0.5～3wt%, hydramine is 0.5～5% in the finished product.
2, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that in the step 1), and is at first that sodium hydroxide is soluble in water, is heated to 80～130 ℃, adds aluminium hydroxide then; Under said temperature, react and to obtain the liquid sodium aluminate in 2～6 hours.
3,, it is characterized in that preferred 90～110 ℃ of temperature of reaction in the step 1), preferred 3～5 hours of reaction times as the preparation method of low-alkaline liquid accelerating agent as described in the claim 2.
4, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that step 2) in preferred 5: 1～3.5: 1 of the mass ratio of sodium aluminate and properties-correcting agent.
5, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that step 2) in the liquid sodium aluminate is being not less than 1000S
-1High-shear state add in the properties-correcting agent down, and sustained reaction 0.5～2 hour.
6, as the preparation method of low-alkaline liquid accelerating agent as described in claim 1 or 4 or 5, it is characterized in that step 2) in the liquid sodium aluminate is being added in the process of properties-correcting agent, water adds when gel occurring, treat that gel dissolving back continuation adds remaining liquid aluminium acid sodium solution, makes the modified liquid sodium aluminate.
7, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that preferred 1: 5～1: 6 of the mass ratio of modified liquid sodium aluminate and alum liquor in the step 3).
8, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that dripping in the step 3) and should be not less than 3000S
-1Shear conditions under carry out, the dropping time is 30～90 minutes; Whole process should be carried out under 10～30 ℃ temperature; After being added dropwise to complete, solution temperature is slowly risen to 50～60 ℃, be incubated 1～2 hour then, obtain brown xanchromatic clear solution.
9,, it is characterized in that step 3) drips preferred 40～60 minutes of time as the preparation method of low-alkaline liquid accelerating agent as described in the claim 8.
10, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that the hydramine in the step 4) is selected from trolamine, diethanolamine or Monoethanolamine MEA BASF; Hydroxycarboxylic acid is selected from formic acid, lactic acid or oxyacetic acid.
11, the preparation method of low-alkaline liquid accelerating agent according to claim 1 is characterized in that preferred diethanolamine of hydramine or trolamine in the step 4).
12, adopt the application method of the low-alkaline liquid accelerating agent of any described method preparation of claim 1 to 13, it is characterized in that according to routine liquid accelerator being joined in the sprayed concrete mixture and prepare sprayed concrete, its usage quantity is 5～8% of a cement consumption.
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| CN102198968A (en) * | 2010-03-25 | 2011-09-28 | 崔涛 | Heavy metal and arsenic ion complexing agent and preparation method and using method thereof |
| CN102219426A (en) * | 2011-04-15 | 2011-10-19 | 中铁隧道集团有限公司 | Low-alkaline liquid accelerating agent and preparation method thereof |
| CN102219425A (en) * | 2011-04-15 | 2011-10-19 | 中铁隧道集团有限公司 | Alkali-free liquid accelerating agent and preparation method thereof |
| CN102786256A (en) * | 2012-09-05 | 2012-11-21 | 江苏南瓷绝缘子有限公司 | Liquid accelerator for sprayed concrete and application thereof |
| CN103396027A (en) * | 2013-07-25 | 2013-11-20 | 北京市建筑工程研究院有限责任公司 | Preparation method of novel alkali-free liquid accelerator |
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| AU723970B2 (en) * | 1996-06-14 | 2000-09-07 | Construction Research & Technology Gmbh | Concrete spraying additives |
| CN1559962A (en) * | 2004-02-16 | 2005-01-05 | 衡 王 | Manufacture of liquid non-alkali accelerating agent |
| CN100386281C (en) * | 2006-12-08 | 2008-05-07 | 王衡 | Powdery alkali-free quick-coagulant |
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| CN102219426B (en) * | 2011-04-15 | 2013-02-20 | 中铁隧道集团有限公司 | Low-alkaline liquid accelerating agent and preparation method thereof |
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