CN108101403A - A kind of preparation method of environment-friendly type alkali-free liquid accelerator - Google Patents
A kind of preparation method of environment-friendly type alkali-free liquid accelerator Download PDFInfo
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- CN108101403A CN108101403A CN201711468534.7A CN201711468534A CN108101403A CN 108101403 A CN108101403 A CN 108101403A CN 201711468534 A CN201711468534 A CN 201711468534A CN 108101403 A CN108101403 A CN 108101403A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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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
- C04B2103/12—Set accelerators
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of environment-friendly type alkali-free liquid accelerator.The preparation method of the present invention is by carrying out being copolymerized obtained suspension stabilizer acrylamide and unsaturated acids, use it for preparing the synthesis of alkali-free liquid accelerator again, accelerator is optimized by introducing high-molecular copolymer, improve the coherency of liquid accelerator, the effective generation for inhibiting precipitation, the stability of mother liquor storage is substantially increased, stability can reach 1 year or more.Environment-friendly type alkali-free liquid accelerator prepared by the present invention is non-corrosive to construction worker's skin, pollution-free to production environment, belongs to green product without environmental pollution.
Description
Technical field
The invention belongs to building material technical fields, and in particular to a kind of preparation side of environment-friendly type alkali-free liquid accelerator
Method.
Background technology
With large-scale mining, tunnel excavation and network of highways and the acceleration of railway network engineering construction so that speed
Solidifying agent dosage greatly increases, and higher requirement is also proposed to the performance quality of accelerator.Conventional powdered accelerator product can only
Construct applied to dry pressure spray process, and there are solution rate it is slow, be not easy to be uniformly dispersed the defects of.
At present, the development trend of gunite concrete accelerator is changed from traditional solid powdery to liquid, and
Low alkali, alkali-free just progressively substitute traditional accelerator.There are alkali content height, later strengths for the liquid accelerator that the country uses at present
The problems such as loss is big, maturing is impervious poor.The high environmental pollution of alkali content is serious, and big, coagulation is injured to construction personnel
The problems such as soil property amount is unstable in order to improve injury of the accelerator to constructor and concrete quality, develops a kind of environment-friendly type
Alkali-free liquid accelerator is of great significance.
The content of the invention
It is an object of the invention to overcome prior art defect, a kind of preparation side of environment-friendly type alkali-free liquid accelerator is provided
Method.
Technical scheme is as follows：
A kind of preparation method of environment-friendly type alkali-free liquid accelerator, includes the following steps：
(1) by acrylamide aqueous solution, unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides aqueous solution, initiator solution and molecule
Amount conditioning agent aqueous solution, which is instilled in water, to be reacted, and reaction temperature is 50-90 DEG C, and time for adding 0.2-6.0h is added dropwise
After add in accelerating agent, keep the temperature 0-3.0h, obtain suspension stabilizer；The total amount of water causes the quality of the suspension stabilizer used in the step
Concentration is 5-40%, the mass ratio of acrylamide solution and unsaturated acids solution is 1: 0.2-1, and the dosage of initiator is propylene
The 0.5-3.0% of the gross mass of amide aqueous solution and unsaturated carboxylic acid or the solute in unsaturated carboxylic acid anhydrides aqueous solution, molecular weight
The dosage of conditioning agent is acrylamide aqueous solution and the gross mass of unsaturated carboxylic acid or the solute in unsaturated carboxylic acid anhydrides aqueous solution
0.2-3.0%, the dosage of accelerating agent is in acrylamide aqueous solution and unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides aqueous solution
The 0.1-1.0% of the gross mass of solute；Above-mentioned unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides are maleic anhydride, acrylic acid, methyl-prop
At least one of olefin(e) acid, fumaric acid, itaconic acid；
(2) hydramine and acid are reacted, 50-90 DEG C of reaction temperature, adds catalyst, reaction time 1-4h is obtained
To modified hydramine；The mass ratio of hydramine and acid is 1: 0.3-1, and the dosage of catalyst is hydramine and the 0.3- of the gross mass of acid
4.0%；At least one of in the step, above-mentioned hydramine is monoethanolamine, diethanol amine, triethanolamine and triisopropanolamine,
Above-mentioned acid is dihydromethyl propionic acid and/or dimethylolpropionic acid；
(3) by weight, suspension stabilizer and 1-10 parts of pH adjusting agents made from 0.2-3.0 parts of steps (1) are added
Enter and be stirred into water, reaction temperature is 10-60 DEG C, adds 30-60 parts of aluminum sulfate, 1-20 parts are added after 0.2-2.0h
Modified hydramine, reacts 0.2-1h, obtains the environment-friendly type alkali-free liquid accelerator made from step (2)；Water is total used in the step
Amount is so that the mass concentration of the environment-friendly type alkali-free liquid accelerator is 40-70%.
In a preferred embodiment of the invention, the initiator is ammonium persulfate and/or potassium peroxydisulfate.
In a preferred embodiment of the invention, the molecular weight regulator is thioacetic acid, mercaptopropionic acid, sulfydryl
At least one of ethyl alcohol, isopropanol and lauryl mercaptan.
In a preferred embodiment of the invention, the accelerating agent is dihydroxytartaric acid, potassium hydrogen tartrate, winestone
At least one of sour hydrogen sodium.
In a preferred embodiment of the invention, the catalyst is p-methyl benzenesulfonic acid and/or the concentrated sulfuric acid.
The beneficial effects of the invention are as follows：
1st, preparation method of the invention is copolymerized obtained suspension stabilizer by the way that acrylamide and unsaturated acids are carried out, then will
It is used to prepare the synthesis of alkali-free liquid accelerator, and accelerator is optimized by introducing high-molecular copolymer, improves liquid
The coherency of body accelerator effectively inhibits the generation of precipitation, substantially increases the stability of mother liquor storage, stability can
Reach 1 year or more.
2nd, the environment-friendly type alkali-free liquid accelerator for preparing of the present invention is non-corrosive to construction worker's skin, to production environment without
Pollution, belongs to green product without environmental pollution.
3rd, modified hydramine is made by react hydramine and acid in preparation method method of the present invention, then is applied to
In the synthesis of alkali-free liquid accelerator, the early strength and later strength of concrete can be improved.
4th, suspension stabilizer prepared by preparation method of the present invention adds in accelerating agent after copolymerization, the introducing of the accelerating agent
The conversion ratio of copolyreaction can not only be improved, moreover it is possible to the initial set of effective control alkali-free liquid accelerator and final setting time.
5th, environment-friendly type alkali-free liquid accelerator prepared by the present invention can adapt to various cement, meet cement setting time
It is required that it can be widely applied in the construction of gunite concrete.
Specific embodiment
Technical scheme is further detailed and described below by way of specific embodiment.
Embodiment 1
(1) preparation of suspension stabilizer：By acrylamide aqueous solution (its acrylamide 100.00g, water 80.00g), Malaysia
Acid anhydrides and acrylic acid aqueous solution (wherein maleic anhydride 22.00g, acrylic acid 13.00g and water 20.00g, ammonium persulfate aqueous solution
(wherein ammonium persulfate 1.20g, water 20.00g) and thioacetic acid aqueous solution (wherein thioacetic acid 0.90g, water 20.00g) instill
It is reacted in 160.00g water, is warming up to 70 DEG C of reactions, time for adding 5.0h adds in 0.50g dihydroxy base liquors after being added dropwise
Stone acid, keeps the temperature 3.0h, obtains suspension stabilizer；
(2) preparation of modified hydramine：100.00g diethanol amine and 45.00g dihydromethyl propionic acids are uniformly mixed, heated up
To 65 DEG C, 2.00g p-methyl benzenesulfonic acid is added, reacts 2h, obtains modified hydramine；
(3) stock up by following mass ratio：
1.60g suspension stabilizers obtained above and 3.00g p-methyl benzenesulfonic acid are added in 60.00g water and are stirred,
Reaction temperature is 30 DEG C, then 40.00g is added to enter aluminum sulfate, and modified hydramine, reaction made from 10.00g appeals are added after 1.0h
0.5h obtains a kind of environment-friendly type alkali-free liquid accelerator KZJ-1.
Embodiment 2
(1) preparation of suspension stabilizer：By acrylamide aqueous solution (its acrylamide 100.00g, water 80.00g), methyl
Acrylic acid and maleic anhydride aqueous solution (wherein methacrylic acid 32.00g, maleic anhydride 20.00g and water 20.00g, potassium peroxydisulfate
Aqueous solution (wherein potassium peroxydisulfate 1.80g, water 20.00g) and thioacetic acid aqueous solution (wherein thioacetic acid 0.80g, water
It 20.00g) instills in 130.00g water and is reacted, be warming up to 60 DEG C of reactions, time for adding 4.0h is added in after being added dropwise
0.60g potassium hydrogen tartrates keep the temperature 2.0h, obtain suspension stabilizer；
(2) preparation of modified hydramine：100.00g triethanolamines and 40.00g dimethylolpropionic acids are uniformly mixed, heated up
To 70 DEG C, the 2.50g concentrated sulfuric acids are added, react 3h, obtain modified hydramine；
(3) stock up by following mass ratio：
0.80g suspension stabilizers obtained above and 4.00g citric acids are added in 60.00g water and are stirred, is reacted
Temperature is 40 DEG C, then 30.00g is added to enter aluminum sulfate, and modified hydramine made from 6.00g appeals is added after 1.0h, 0.5h is reacted, obtains
To a kind of environment-friendly type alkali-free liquid accelerator KZJ-2.
Embodiment 3
(1) preparation of suspension stabilizer：By acrylamide aqueous solution (its acrylamide 100.00g, water 80.00g), rich horse
(wherein fumaric acid 18.00g, methacrylic acid 40.00g and water 20.00g, ammonium persulfate are water-soluble with metering system aqueous acid for acid
Liquid (wherein ammonium persulfate 1.80g, water 20.00g) and thioacetic acid aqueous solution (wherein thioacetic acid 1.00g, water 20.00g) drop
Enter and reacted in 130.00g water, be warming up to 65 DEG C of reactions, time for adding 3.0h adds in 1.00g tartaric acid after being added dropwise
Hydrogen sodium keeps the temperature 1.0h, obtains suspension stabilizer；
(2) preparation of modified hydramine：100.00g monoethanolamines and 50.00g dihydromethyl propionic acids are uniformly mixed, heated up
To 70 DEG C, 4.00g p-methyl benzenesulfonic acid is added, reacts 1h, obtains modified hydramine；
(3) stock up by following mass ratio：
1.20g suspension stabilizers obtained above and 5.00g tartaric acid are added in 60.00g water and are stirred, is reacted
Temperature is 45 DEG C, then 36.00g is added to enter aluminum sulfate, and modified hydramine made from 12.00g appeals is added after 1.5h, reacts 0.5h,
Obtain a kind of environment-friendly type alkali-free liquid accelerator KZJ-3.
Embodiment 4
(1) preparation of suspension stabilizer：By acrylamide aqueous solution (its acrylamide 100.00g, water 80.00g), clothing health
(wherein itaconic acid 11.00g, acrylic acid 36.00g and water 20.00g, ammonium persulfate aqueous solution is (wherein with acrylic acid aqueous solution for acid
Ammonium persulfate 2.00g, water 20.00g) and mercaptoethanol aqueous solution (wherein mercaptoethanol 1.00g, water 20.00g) instillation
It is reacted in 260.00g water, is warming up to 80 DEG C of reactions, time for adding 2.0h adds in 1.10g dihydroxy base liquors after being added dropwise
Stone acid, keeps the temperature 0.5h, obtains suspension stabilizer；
(2) preparation of modified hydramine：100.00g triisopropanolamines and 60.00g dimethylolpropionic acids are uniformly mixed, risen
Temperature adds the 3.00g concentrated sulfuric acids to 60 DEG C, reacts 4h, obtains modified hydramine；
(3) stock up by following mass ratio：
1.00g suspension stabilizers obtained above and 5.00g salicylic acids are added in 60.00g water and are stirred, is reacted
Temperature is 30 DEG C, then 33.00g is added to enter aluminum sulfate, and modified hydramine made from 10.00g appeals is added after 1.0h, reacts 0.5h,
Obtain a kind of environment-friendly type alkali-free liquid accelerator KZJ-4.
Embodiment 5
(1) prepared by suspension stabilizer：By acrylamide aqueous solution (its acrylamide 100.00g, water 80.00g), methyl-prop
Olefin(e) acid and acrylic acid aqueous solution (wherein methacrylic acid 22.00g, acrylic acid 36.00g and water 20.00g, ammonium persulfate aqueous solution
(wherein ammonium persulfate 1.60g, water 20.00g) and isopropanol water solution (wherein isopropanol 0.70g, water 20.00g) instill
It is reacted in 460.00g water, is warming up to 90 DEG C of reactions, time for adding 1.0h adds in 0.40g dihydroxy base liquors after being added dropwise
Stone acid, keeps the temperature 1.5h, obtains suspension stabilizer；
(2) preparation of modified hydramine：100.00g triethanolamines and 70.00g dihydromethyl propionic acids are uniformly mixed, heated up
To 75 DEG C, 5.00g p-methyl benzenesulfonic acid is added, reacts 3h, obtains modified hydramine；
(3) stock up by following mass ratio：
2.20g suspension stabilizers obtained above and 7.00g ethanedioic acids are added in 60.00g water and are stirred, is reacted
Temperature is 25 DEG C, then 43.00g is added to enter aluminum sulfate, and modified hydramine made from 15.00g appeals is added after 1.0h, reacts 0.4h,
Obtain a kind of environment-friendly type alkali-free liquid accelerator KZJ-5.
Environment-friendly type alkali-free liquid accelerator obtained by embodiment 1 to embodiment 5 is tested, selects three representativenesses
Cement is tested, cement be respectively 42.5 Portland cements of Fujian good fortune P.O, 42.5 Portland cements of conch P.O,
42.5 Portland cements of Taurus P.O.According to JC477-2005《Gunite concrete accelerator》To gained environment-friendly type alkali-free
Liquid accelerator carries out cement paste condensation water time and strength of cement mortar experiment.Wherein accelerator dosage is according to cement weight
Percentage calculation.
Cement paste setting time tests
Cement 400
Water 160
Strength of cement mortar is tested
Cement 900
Normal sand 1350
Water 450
Accelerator is added according to the 5% of cement weight in cement slurry, while above-mentioned water consumption contains liquid accelerator
In contained water.With presently commercially available alkali-free liquid accelerator (sample 1) as a comparison, cement paste setting time, sand have been carried out
Slurry intensity and stability are tested.Result of the test such as table 1 and 2.
1 cement paste setting time test result of table
2 strength of cement mortar of table is tested and stability
The presetting period of environment-friendly type alkali-free liquid accelerator of the invention and final setting time be all as can be seen from Table 1 and Table 2
More shorter than commercially available alkali-free liquid accelerator, 1d compression strength and 28d compressive strength rate highers, stability are more preferable.
Those of ordinary skill in the art understand, when technical scheme changes in following ranges, remain able to
To same as the previously described embodiments or similar technique effect, protection scope of the present invention is still fallen within：
A kind of preparation method of environment-friendly type alkali-free liquid accelerator, includes the following steps：
(1) by acrylamide aqueous solution, unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides aqueous solution, initiator solution and molecule
Amount conditioning agent aqueous solution, which is instilled in water, to be reacted, and reaction temperature is 50-90 DEG C, and time for adding 0.2-6.0h is added dropwise
After add in accelerating agent, keep the temperature 0-3.0h, obtain suspension stabilizer；The total amount of water causes the quality of the suspension stabilizer used in the step
Concentration is 5-40%, the mass ratio of acrylamide solution and unsaturated acids solution is 1: 0.2-1, and the dosage of initiator is propylene
The 0.5-3.0% of the gross mass of amide aqueous solution and unsaturated carboxylic acid or the solute in unsaturated carboxylic acid anhydrides aqueous solution, molecular weight
The dosage of conditioning agent is acrylamide aqueous solution and the gross mass of unsaturated carboxylic acid or the solute in unsaturated carboxylic acid anhydrides aqueous solution
0.2-3.0%, the dosage of accelerating agent is in acrylamide aqueous solution and unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides aqueous solution
The 0.1-1.0% of the gross mass of solute；Above-mentioned unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides are maleic anhydride, acrylic acid, methyl-prop
At least one of olefin(e) acid, fumaric acid, itaconic acid；
(2) hydramine and acid are reacted, 50-90 DEG C of reaction temperature, adds catalyst, reaction time 1-4h is obtained
To modified hydramine；The mass ratio of hydramine and acid is 1: 0.3-1, and the dosage of catalyst is hydramine and the 0.3- of the gross mass of acid
4.0%；At least one of in the step, above-mentioned hydramine is monoethanolamine, diethanol amine, triethanolamine and triisopropanolamine,
Above-mentioned acid is dihydromethyl propionic acid and/or dimethylolpropionic acid；
(3) by weight, suspension stabilizer and 1-10 parts of pH adjusting agents made from 0.2-3.0 parts of steps (1) are added
Enter and be stirred into water, reaction temperature is 10-60 DEG C, adds 30-60 parts of aluminum sulfate, 1-20 parts are added after 0.2-2.0h
Modified hydramine, reacts 0.2-1h, obtains the environment-friendly type alkali-free liquid accelerator made from step (2)；Water is total used in the step
Amount is so that the mass concentration of the environment-friendly type alkali-free liquid accelerator is 40-70%.
The initiator is ammonium persulfate and/or potassium peroxydisulfate.The molecular weight regulator is thioacetic acid, sulfydryl third
At least one of acid, mercaptoethanol, isopropanol and lauryl mercaptan.The accelerating agent for dihydroxytartaric acid, potassium hydrogen tartrate,
At least one of sodium hydrogen tartrate.The catalyst is p-methyl benzenesulfonic acid and/or the concentrated sulfuric acid.
The foregoing is only a preferred embodiment of the present invention, therefore cannot limit the scope that the present invention is implemented according to this, i.e.,
According to the equivalent changes and modifications that the scope of the claims of the present invention and description are made, all should still belong in the range of the present invention covers.
Claims (5)
1. a kind of preparation method of environment-friendly type alkali-free liquid accelerator, it is characterised in that：Include the following steps：
(1) by acrylamide aqueous solution, unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides aqueous solution, initiator solution and molecular weight tune
Section agent aqueous solution, which is instilled in water, to be reacted, and reaction temperature is 50-90 DEG C, time for adding 0.2-6.0h, is added after being added dropwise
Enter accelerating agent, keep the temperature 0-3.0h, obtain suspension stabilizer；The total amount of water causes the mass concentration of the suspension stabilizer used in the step
For 5-40%, the mass ratio of acrylamide solution and unsaturated acids solution is 1: 0.2-1, and the dosage of initiator is acrylamide
The 0.5-3.0% of the gross mass of aqueous solution and unsaturated carboxylic acid or the solute in unsaturated carboxylic acid anhydrides aqueous solution, molecular-weight adjusting
The dosage of agent is acrylamide aqueous solution and the gross mass of unsaturated carboxylic acid or the solute in unsaturated carboxylic acid anhydrides aqueous solution
0.2-3.0%, the dosage of accelerating agent is molten in acrylamide aqueous solution and unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides aqueous solution
The 0.1-1.0% of the gross mass of matter；Above-mentioned unsaturated carboxylic acid or unsaturated carboxylic acid anhydrides are maleic anhydride, acrylic acid, metering system
At least one of acid, fumaric acid, itaconic acid；
(2) hydramine and acid are reacted, 50-90 DEG C of reaction temperature, adds catalyst, reaction time 1-4h is changed
Property hydramine；The mass ratio of hydramine and acid is 1: 0.3-1, and the dosage of catalyst is hydramine and the 0.3-4.0% of the gross mass of acid；It should
In step, above-mentioned hydramine is at least one of monoethanolamine, diethanol amine, triethanolamine and triisopropanolamine, and above-mentioned acid is
Dihydromethyl propionic acid and/or dimethylolpropionic acid；
(3) by weight, suspension stabilizer and 1-10 parts of pH adjusting agents made from 0.2-3.0 parts of steps (1) are added to
It is stirred in water, reaction temperature is 10-60 DEG C, adds 30-60 parts of aluminum sulfate, 1-20 parts of steps are added after 0.2-2.0h
(2) modified hydramine, reacts 0.2-1h, obtains the environment-friendly type alkali-free liquid accelerator made from；The total amount of water makes used in the step
The mass concentration for obtaining the environment-friendly type alkali-free liquid accelerator is 40-70%.
2. preparation method as described in claim 1, it is characterised in that：The initiator is ammonium persulfate and/or potassium peroxydisulfate.
3. preparation method as described in claim 1, it is characterised in that：The molecular weight regulator is thioacetic acid, sulfydryl third
At least one of acid, mercaptoethanol, isopropanol and lauryl mercaptan.
4. preparation method as described in claim 1, it is characterised in that：The accelerating agent is dihydroxytartaric acid, hydrogen tartrate
At least one of potassium, sodium hydrogen tartrate.
5. preparation method as described in claim 1, it is characterised in that：The catalyst is p-methyl benzenesulfonic acid and/or the concentrated sulfuric acid.
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| CN108793811A (en) * | 2018-08-16 | 2018-11-13 | 科之杰新材料集团有限公司 | A kind of preparation method of the enhanced alkali-free liquid accelerator of durability |
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| CN112608065B (en) * | 2019-12-13 | 2022-07-15 | 科之杰新材料集团(贵州)有限公司 | Liquid alkali-free accelerator for sprayed concrete and preparation method thereof |
| CN111646728A (en) * | 2020-07-01 | 2020-09-11 | 中建材中岩科技有限公司 | Quick-setting high-strength alkali-free liquid accelerator |
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