CN106587709B - Polycarboxylate water-reducer and preparation method thereof - Google Patents
Polycarboxylate water-reducer and preparation method thereof Download PDFInfo
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- CN106587709B CN106587709B CN201611143026.7A CN201611143026A CN106587709B CN 106587709 B CN106587709 B CN 106587709B CN 201611143026 A CN201611143026 A CN 201611143026A CN 106587709 B CN106587709 B CN 106587709B
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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
- 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
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The invention discloses a kind of polycarboxylate water-reducer and preparation method thereof, polycarboxylate water-reducer includes the raw material of following parts by weight：40~60 parts of alkyl phenol polyoxyethylene ether, 25~35 parts of isoamyl alcohol polyoxyethylene ether, 10~15 parts of cinnamic acid, 10~15 parts of octenyl succinic acid anhydride, 5~10 parts of cinnamic acid, 5~10 parts of methacrylic acid, 3~8 parts of isopropanol, 3~8 parts of sodium peroxydisulfate and 0.5~2 part of ascorbic acid.Polycarboxylate water-reducer of the invention is lower than common polycarboxylate water-reducer volume, and can all show that high water reducing rate, the scope of application are wider, and concrete collapse-proof is good in the case where different water-binder ratios, more environmentally-friendly advantage.The polycarboxylate water-reducer of preparation method preparation of the invention is wider to the adaptability of cement, keeps system more stable, can be reduced the use of air entraining agent, concrete shrinkage value is made to be less than ordinary water-reducing agent.
Description
Technical field
The present invention relates to concrete admixture fields.It is more particularly related to a kind of polycarboxylate water-reducer and its
Preparation method.
Background technique
Water-reducing agent can keep cement paste, mortar and concrete work degree constant and substantially reduce its mixing water amount
Additive can significantly improve concrete strength, improve the frost resistance of concrete, impervious or reduction cement consumption.Existing market
Above common several water-reducing agents are：Lignin sulfonic acid sodium salt water-reducing agent, naphthalene series high-efficiency water-reducing agent, aliphatic high-efficiency water reducing agent, ammonia
Base high efficiency water reducing agent, high performance water reducing agent of polyocarboxy acid etc..It is commonly subtracting for representative that polycarboxylate high performance water-reducing agent, which is after calcium lignosulfonate,
Aqua and using naphthalene system as the third generation high-performance water reducing agent that grows up after the high efficiency water reducing agent of representative is at present in the world most
Forward position, a kind of high efficiency water reducing agent that scientific and technological content highest, application prospect is best, comprehensive performance is optimal.
The research and development of polycarboxylate water-reducer should be many-sided comprehensive from concrete performance, price, environmental protection, sustainable development etc.
Consider, further develops towards high performance, multifunction, ecology direction, cheap, the simple polycarboxylic-acid of synthesis technology
The research of water-reducing agent all has great importance to the progress of China's concrete material, construction project, and polycarboxylate water-reducer is mixed
Measure low, the slump is kept, but people are also constantly looking for the higher polycarboxylate water-reducer of water-reducing rate in practical applications, simultaneously
The low-dosage of polycarboxylate water-reducer is very sensitive in water-cement ratio hour, and has shown more high water reducing rate, and when water-cement ratio is big,
Water-reducing rate and its variation it is just less obvious so that polycarboxylate water-reducer volume it is low advantage it is in actual use and unknown
It is aobvious, therefore need to find that a kind of water-reducing rate is higher, high water reducing rate, the scope of application can be all shown in the case where different water-binder ratios
Wider array of polycarboxylate water-reducer and the preparation method that such high-performance polycarboxylic acids water reducing agent can be made.
Summary of the invention
It is an object of the invention to solve the above problems, and provide the advantages of will be described later.
It is a still further object of the present invention to provide a kind of polycarboxylate water-reducers, by alkyl phenol polyoxyethylene ether and prenol
The copolymerization such as polyoxyethylene ether macromolecular combination cinnamic acid, octenyl succinic acid anhydride, cinnamic acid and methacrylic acid
Obtained polycarboxylate water-reducer is lower than common polycarboxylate water-reducer volume, and can all show in the case where different water-binder ratios
High water reducing rate, the scope of application are wider, and concrete collapse-proof is good, more environmentally-friendly advantage.
It is a still further object of the present invention to provide a kind of preparation method of polycarboxylate water-reducer, by by various raw materials by several times
The mode that addition is incorporated in 80 DEG C and 45 DEG C step heat preservations keeps the polycarboxylate water-reducer of preparation wider to the adaptability of cement, makes
System is more stable, can be reduced the use of air entraining agent, is less than commonly using the concrete shrinkage value of polycarboxylate water-reducer of the present invention
Water-reducing agent.
In order to realize these purposes and other advantages according to the present invention, a kind of polycarboxylate water-reducer is provided, including with
The raw material of lower parts by weight：
It is 40~60 parts of alkyl phenol polyoxyethylene ether, 25~35 parts of isoamyl alcohol polyoxyethylene ether, 10~15 parts of cinnamic acid, pungent
10~15 parts of alkenyl succinic anhydride, 5~10 parts of cinnamic acid, 5~10 parts of methacrylic acid, 3~8 parts of isopropanol, mistake
3~8 parts of sodium sulphate and 0.5~2 part of ascorbic acid.
It preferably, further include the raw material of following parts by weight：0.5~1 part of modified rosin resin and propylene glycol monostearate
0.5~1 part of ester.
Preferably, the molecular weight of isoamyl alcohol polyoxyethylene ether is 800~1000, the molecule of alkyl phenol polyoxyethylene ether
Amount is 600~1000.
Preferably, according to parts by weight, 50 parts of alkyl phenol polyoxyethylene ether, 30 parts of isoamyl alcohol polyoxyethylene ether, meat
12 parts of cinnamic acid, 12 parts of octenyl succinic acid anhydride, 8 parts of cinnamic acid, 6 parts of methacrylic acid, 5 parts of isopropanol, persulfuric acid
5 parts of sodium and 1 part of ascorbic acid.
The present invention also provides a kind of preparation methods of polycarboxylate water-reducer, include the following steps：
Step 1：At normal temperature, according to parts by weight, 40~60 parts of alkyl phenol polyoxyethylene ether and prenol polyoxy are taken
50~80 parts of water is added after 25~35 parts of vinethene to be dissolved to obtain the first solution；
Step 2：According to parts by weight, by 10~15 parts of cinnamic acid, 10~15 parts of octenyl succinic acid anhydride, 3- phenyl -2-
5~10 parts of acrylic acid, it is molten to obtain second for the water of 20~40 parts of addition after 5~10 parts and 1 part of ascorbic acid mixing of methacrylic acid
Second solution is added dropwise into first solution for liquid, after obtain third solution；
Step 3：According to parts by weight, 3~8 parts of the isopropanol water for being added 10~20 parts are taken to obtain the 4th solution, the 5th is molten
Include 3~8 parts of sodium peroxydisulfates and 5~10 parts of water in liquid, the third solution is heated to starting to be added dropwise after 80 DEG C described the
Five solution after 5~10min is added dropwise start that the 4th solution is added dropwise, the 6th solution are obtained after dripping；
Step 4：6th solution is kept the temperature into 0.5~1h at 80 DEG C, after being then cooled to 45 DEG C of 1~1.5h of heat preservation
Obtain polycarboxylate water-reducer.
It preferably, according to parts by weight, further include modified rosin resin 0.5 in the 5th solution described in the step 3
~1 part and 0.5~2 part of propylene glycol monostearate.
Preferably, the rate of addition of the 4th solution described in the step 3 is the rate of addition of the 5th solution
1.5 again.
Preferably, after the 6th solution being kept the temperature at 80 DEG C in the step 4, adjusted with sodium hydroxide described in
The pH of 6th solution is 5.5~6.5, and after being cooled to 45 DEG C of 1~1.5h of heat preservation, the pH of the 6th solution is adjusted with sodium hydroxide
It is 6.5~7.5.
Preferably, mixing speed when the 6th solution being kept the temperature 0.5~1h at 80 DEG C in the step 4 is
200r/min, mixing speed when being then cooled to 45 DEG C of 1~1.5h of heat preservation are 400r/min.
Preferably, the step 4 is to use the 6th solution at 80 DEG C power to keep the temperature for the microwave of 500W
0.5h, be then cooled to 45 DEG C use power for 250W microwave keep the temperature 0.5h after obtain polycarboxylate water-reducer.
The present invention is include at least the following beneficial effects：
In polycarboxylate water-reducer formula of the invention, alkyl phenol polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether are divided greatly
Son is used as matrix, in conjunction with cinnamic acid, ascorbic acid, octenyl succinic acid anhydride, cinnamic acid and methacrylic acid etc.
A variety of acrylic acid or acid anhydrides are copolymerized as monomer, and using sodium peroxydisulfate as initiator, isopropanol obtains poly- carboxylic as chain-transferring agent
Sour water-reducing agent, system combine it is more stable so that the steric hindrance of polycarboxylic acids molecule is larger, smaller volume water-cement ratio hour very
Sensitivity shows more high water reducing rate, and when water-cement ratio is big, the space steric effect that polycarboxylic acids molecular structure is formed is in cement
It is also more significant than common polycarboxylate water-reducer in dispersion, therefore high water reduction can be all shown in the case where different water-binder ratios
Rate, wider to the adaptability of cement, the scope of application is wider, and concrete collapse-proof is good, more environmentally-friendly advantage.
In the preparation method of polycarboxylate water-reducer provided by the invention, 80 DEG C are incorporated in by the way that various raw materials are added by several times
Keep the polycarboxylate water-reducer of preparation wider to the adaptability of cement with the mode of 45 DEG C of step heat preservations, system is more stable, makes band
The bubble for entering concrete had not only been able to satisfy the requirement of air content, but also will not have an adverse effect to performances such as intensity, can be reduced bleed
The use of agent, it is good using the volume stability of polycarboxylate water-reducer of the present invention, so that concrete shrinkage value is less than ordinary water-reducing agent.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
Embodiment 1
Polycarboxylate water-reducer, the raw material including following parts by weight：40 parts of alkyl phenol polyoxyethylene ether, prenol polyoxy second
25 parts of alkene ether, 10 parts of cinnamic acid, 10 parts of octenyl succinic acid anhydride, 5 parts of cinnamic acid, 5 parts of methacrylic acid, isopropyl
3 parts of alcohol, 3 parts of sodium peroxydisulfate and 0.5 part of ascorbic acid.
Embodiment 2
Polycarboxylate water-reducer, the raw material including following parts by weight：60 parts of alkyl phenol polyoxyethylene ether, prenol polyoxy second
It is 35 parts of alkene ether, 15 parts of cinnamic acid, 15 parts of octenyl succinic acid anhydride, 10 parts of cinnamic acid, 10 parts of methacrylic acid, different
8 parts of propyl alcohol, 8 parts of sodium peroxydisulfate and 2 parts of ascorbic acid.
Embodiment 3
Polycarboxylate water-reducer, the raw material including following parts by weight：50 parts of alkyl phenol polyoxyethylene ether, prenol polyoxy second
30 parts of alkene ether, 12 parts of cinnamic acid, 12 parts of octenyl succinic acid anhydride, 8 parts of cinnamic acid, 6 parts of methacrylic acid, isopropyl
5 parts of alcohol, 5 parts of sodium peroxydisulfate and 1 part of ascorbic acid.
Embodiment 4
Step 1：At normal temperature, according to parts by weight, 40 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
50 parts of water is added after 25 parts of ether to be dissolved to obtain the first solution.
Step 2：According to parts by weight, by 10 parts of cinnamic acid, 10 parts of octenyl succinic acid anhydride, cinnamic acid 5
Part, 20 parts of water is added after 5 parts and 0.5 part of ascorbic acid mixing of methacrylic acid and obtains the second solution, to first solution
It is interior that second solution is added dropwise, after obtain third solution.
Step 3：According to parts by weight, it takes 3 parts of the isopropanol water for being added 10 parts to obtain the 4th solution, is wrapped in the 5th solution
3 parts of sodium peroxydisulfates and 5 parts of water are included, the third solution is heated to start to be added dropwise the 5th solution after 80 DEG C, is added dropwise
Start that the 4th solution is added dropwise after 5min, the 6th solution is obtained after dripping.
Step 4：6th solution is kept the temperature into 0.5h at 80 DEG C, obtains poly- carboxylic after being then cooled to 45 DEG C of heat preservation 1h
Sour water-reducing agent.
Embodiment 5
Step 1：At normal temperature, according to parts by weight, 60 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
80 parts of water is added after 35 parts of ether to be dissolved to obtain the first solution.
Step 2：According to parts by weight, by 15 parts of cinnamic acid, 15 parts of octenyl succinic acid anhydride, cinnamic acid 10
Part, 40 parts of water is added after 10 parts and 2 parts of ascorbic acid mixing of methacrylic acid and obtains the second solution, into first solution
Second solution is added dropwise, after obtain third solution.
Step 3：According to parts by weight, it takes 8 parts of the isopropanol water for being added 20 parts to obtain the 4th solution, is wrapped in the 5th solution
8 parts of sodium peroxydisulfates and 10 parts of water are included, the third solution is heated to start to be added dropwise the 5th solution after 80 DEG C, is added dropwise
Start that the 4th solution is added dropwise after 10min, the 6th solution is obtained after dripping.
Step 4：6th solution is kept the temperature into 1h at 80 DEG C, obtains poly- carboxylic after being then cooled to 45 DEG C of heat preservation 1.5h
Sour water-reducing agent.
Embodiment 6
Step 1：At normal temperature, according to parts by weight, 50 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
60 parts of water is added after 30 parts of ether to be dissolved to obtain the first solution.
Step 2：According to parts by weight, by 12 parts of cinnamic acid, 12 parts of octenyl succinic acid anhydride, cinnamic acid 8
Part, 30 parts of water is added after 6 parts and 1 part of ascorbic acid mixing of methacrylic acid and obtains the second solution, into first solution
Second solution is added dropwise, after obtain third solution.
Step 3：According to parts by weight, it takes 5 parts of the isopropanol water for being added 15 parts to obtain the 4th solution, is wrapped in the 5th solution
5 parts of sodium peroxydisulfates and 8 parts of water are included, the third solution is heated to start to be added dropwise the 5th solution after 80 DEG C, is added dropwise
Start that the 4th solution is added dropwise after 8min, the 6th solution is obtained after dripping.
Step 4：6th solution is kept the temperature into 0.8h at 80 DEG C, is gathered after being then cooled to 45 DEG C of heat preservation 1.2h
Carboxylic acid water reducer.
Embodiment 7
Step 1：At normal temperature, according to parts by weight, 40 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
50 parts of water is added after 25 parts of ether to be dissolved to obtain the first solution, wherein the molecular weight of isoamyl alcohol polyoxyethylene ether is 800
~1000, the molecular weight of alkyl phenol polyoxyethylene ether is 600~1000.Control alkyl phenol polyoxyethylene ether and prenol polyoxy
The molecular weight of vinethene makes the polycarboxylic acids molecule to be formed have the characteristics that low main chain long-chain branch, has more stable comb-type structure.
Step 2：According to parts by weight, by 10 parts of cinnamic acid, 10 parts of octenyl succinic acid anhydride, cinnamic acid 5
Part, 20 parts of water is added after 5 parts and 0.5 part of ascorbic acid mixing of methacrylic acid and obtains the second solution, to first solution
It is interior that second solution is added dropwise, after obtain third solution.Cinnamic acid, octenyl succinic acid anhydride, cinnamic acid,
The addition of methacrylic acid and ascorbic acid etc. keeps active group more various, and active group group is not focusing only on molecule master
It on chain, is more active on the side shoot for grafting in main chain, after polymerizeing with alkyl phenol polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether
Keep macromolecular system more stable so that the steric hindrance for the polycarboxylic acids molecule being subsequently generated is larger, make that branch supports to overhanging
The comb structure of exhibition provides sufficient space arrangement effect for the further dispersion of cement particle.
Step 3：According to parts by weight, it takes 3 parts of the isopropanol water for being added 10 parts to obtain the 4th solution, is wrapped in the 5th solution
3 parts of sodium peroxydisulfates are included, 0.5 part of modified rosin resin, the water that 0.5 part and 5 parts of propylene glycol monostearate is molten by the third
Liquid starts that the 5th solution is added dropwise after being heated to 80 DEG C, after 5min is added dropwise starts that the 4th solution is added dropwise, after dripping
To the 6th solution, wherein the rate of addition of the 4th solution is 1.5 times of the rate of addition of the 5th solution.Control drop
Accelerated energy regulates and controls the length of main chain and branch, keeps the polycarboxylate water-reducer of preparation wider to the adaptability of cement, system is more steady
It is fixed.Wherein, modified rosin resin is air entraining agent, and propylene glycol monostearate is acidproof defoaming agent.
Step 4：It is that 200r/min keeps the temperature 0.5h that 6th solution is adjusted mixing speed at 80 DEG C, uses hydroxide
The pH that sodium adjusts the 6th solution is 5.5, and being then cooled to 45 DEG C of adjusting mixing speeds is after 400r/min keeps the temperature 1h, to use hydrogen
Sodium oxide molybdena adjusts the pH of the 6th solution and obtains polycarboxylate water-reducer for 6.5.Polycarboxylate water-reducer in process of production, gassiness
Amount sometimes up to 8% or so, if directly use is unfavorable to intensity effect, by the side of 80 DEG C and 45 DEG C step heat preservations
Formula can play the role of certain elimination bubble, to decrease the use of defoaming agent and air entraining agent.PH is adjusted stage by stage to be made
Obtained polycarboxylate water-reducer is partial neutral rather than common slant acidity, use are more extensive.
Embodiment 8
Step 1：At normal temperature, according to parts by weight, 60 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
80 parts of water is added after 35 parts of ether to be dissolved to obtain the first solution, wherein the molecular weight of isoamyl alcohol polyoxyethylene ether is 800
~1000, the molecular weight of alkyl phenol polyoxyethylene ether is 600~1000.Control alkyl phenol polyoxyethylene ether and prenol polyoxy
The molecular weight of vinethene makes the polycarboxylic acids molecule to be formed have the characteristics that low main chain long-chain branch, has more stable comb-type structure.
Step 2：According to parts by weight, by 15 parts of cinnamic acid, 15 parts of octenyl succinic acid anhydride, cinnamic acid 10
Part, 40 parts of water is added after 10 parts and 2 parts of ascorbic acid mixing of methacrylic acid and obtains the second solution, into first solution
Second solution is added dropwise, after obtain third solution.Cinnamic acid, octenyl succinic acid anhydride, cinnamic acid, first
The addition of base acrylic acid and ascorbic acid etc. keeps active group more various, and active group group is not focusing only on molecular backbone
On, it is more active on the side shoot for grafting in main chain, makes after polymerizeing with alkyl phenol polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether
Macromolecular system is more stable, so that the steric hindrance for the polycarboxylic acids molecule being subsequently generated is larger, makes flexing outward for branch support
Comb structure for cement particle it is further dispersion provide sufficient space arrangement effect.
Step 3：According to parts by weight, it takes 8 parts of the isopropanol water for being added 20 parts to obtain the 4th solution, is wrapped in the 5th solution
Include 8 parts of sodium peroxydisulfates, 1 part of modified rosin resin, the water that 1 part and 10 parts of propylene glycol monostearate, by the third solution
Start that the 5th solution is added dropwise after being heated to 80 DEG C, after 10min is added dropwise starts that the 4th solution is added dropwise, be obtained after dripping
6th solution, wherein the rate of addition of the 4th solution is 1.5 times of the rate of addition of the 5th solution.Control is added dropwise
Speed can regulate and control the length of main chain and branch, keep the polycarboxylate water-reducer of preparation wider to the adaptability of cement, system is more stable.
Wherein, modified rosin resin is air entraining agent, and propylene glycol monostearate is acidproof defoaming agent.
Step 4：It is that 200r/min keeps the temperature 1h that 6th solution is adjusted mixing speed at 80 DEG C, uses sodium hydroxide
The pH for adjusting the 6th solution is 6.5, and being then cooled to 45 DEG C of adjusting mixing speeds is after 400r/min keeps the temperature 1.5h, to use hydrogen
Sodium oxide molybdena adjusts the pH of the 6th solution and obtains polycarboxylate water-reducer for 7.5.Polycarboxylate water-reducer in process of production, gassiness
Amount sometimes up to 8% or so, if directly use is unfavorable to intensity effect, by the side of 80 DEG C and 45 DEG C step heat preservations
Formula can play the role of certain elimination bubble, to decrease the use of defoaming agent and air entraining agent.PH is adjusted stage by stage to be made
Obtained polycarboxylate water-reducer is neutral rather than common acidity, and use is more extensive.
Embodiment 9
Step 1：At normal temperature, according to parts by weight, 50 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
60 parts of water is added after 30 parts of ether to be dissolved to obtain the first solution, wherein the molecular weight of isoamyl alcohol polyoxyethylene ether is 800
~1000, the molecular weight of alkyl phenol polyoxyethylene ether is 600~1000.Control alkyl phenol polyoxyethylene ether and prenol polyoxy
The molecular weight of vinethene makes the polycarboxylic acids molecule to be formed have the characteristics that low main chain long-chain branch, has more stable comb-type structure.
Step 2：According to parts by weight, by 12 parts of cinnamic acid, 12 parts of octenyl succinic acid anhydride, cinnamic acid 8
Part, 30 parts of water is added after 8 parts and 1 part of ascorbic acid mixing of methacrylic acid and obtains the second solution, into first solution
Second solution is added dropwise, after obtain third solution.Cinnamic acid, octenyl succinic acid anhydride, cinnamic acid, first
The addition of base acrylic acid and ascorbic acid etc. keeps active group more various, and active group group is not focusing only on molecular backbone
On, it is more active on the side shoot for grafting in main chain, makes after polymerizeing with alkyl phenol polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether
Macromolecular system is more stable, so that the steric hindrance for the polycarboxylic acids molecule being subsequently generated is larger, makes flexing outward for branch support
Comb structure for cement particle it is further dispersion provide sufficient space arrangement effect.
Step 3：According to parts by weight, it takes 5 parts of the isopropanol water for being added 15 parts to obtain the 4th solution, is wrapped in the 5th solution
5 parts of sodium peroxydisulfates are included, 0.8 part of modified rosin resin, the water that 0.8 part and 8 parts of propylene glycol monostearate is molten by the third
Liquid starts that the 5th solution is added dropwise after being heated to 80 DEG C, after 8min is added dropwise starts that the 4th solution is added dropwise, after dripping
To the 6th solution, wherein the rate of addition of the 4th solution is 1.5 times of the rate of addition of the 5th solution.Control drop
Accelerated energy regulates and controls the length of main chain and branch, keeps the polycarboxylate water-reducer of preparation wider to the adaptability of cement, system is more steady
It is fixed.Wherein, modified rosin resin is air entraining agent, and propylene glycol monostearate is acidproof defoaming agent.
Step 4：It is that 200r/min keeps the temperature 0.8h that 6th solution is adjusted mixing speed at 80 DEG C, uses hydroxide
The pH that sodium adjusts the 6th solution is 6.0, and being then cooled to 45 DEG C of adjusting mixing speeds is after 400r/min keeps the temperature 1.2h, to use
Sodium hydroxide adjusts the pH of the 6th solution and obtains polycarboxylate water-reducer for 7.0.Polycarboxylate water-reducer in process of production, contains
Tolerance sometimes up to 8% or so, if directly use is unfavorable to intensity effect, by 80 DEG C and 45 DEG C step heat preservations
Mode can play the role of certain elimination bubble, to decrease the use of defoaming agent and air entraining agent.PH is adjusted stage by stage
The polycarboxylate water-reducer partial neutral that makes rather than common slant acidity, use are more extensive.
Embodiment 10
Step 1：At normal temperature, according to parts by weight, 50 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
60 parts of water is added after 30 parts of ether to be dissolved to obtain the first solution, wherein the molecular weight of isoamyl alcohol polyoxyethylene ether is 800
~1000, the molecular weight of alkyl phenol polyoxyethylene ether is 600~1000.
Step 2：According to parts by weight, by 12 parts of cinnamic acid, 12 parts of octenyl succinic acid anhydride, cinnamic acid 8
Part, 30 parts of water is added after 8 parts and 1 part of ascorbic acid mixing of methacrylic acid and obtains the second solution, into first solution
Second solution is added dropwise, after obtain third solution.
Step 3：According to parts by weight, it takes 5 parts of the isopropanol water for being added 15 parts to obtain the 4th solution, is wrapped in the 5th solution
5 parts of sodium peroxydisulfates are included, 0.8 part of modified rosin resin, the water that 0.8 part and 8 parts of propylene glycol monostearate is molten by the third
Liquid starts that the 5th solution is added dropwise after being heated to 80 DEG C, after 8min is added dropwise starts that the 4th solution is added dropwise, after dripping
To the 6th solution, wherein the rate of addition of the 4th solution is 2 times of the rate of addition of the 5th solution.
Step 4：It uses power to keep the temperature 0.5h for the microwave of 500W at 80 DEG C the 6th solution, is then cooled to
45 DEG C use power for 250W microwave keep the temperature 0.5h after obtain polycarboxylate water-reducer.Microwave heat preservation can be further improved polycarboxylic acids
Water-reducing agent water-reducing rate and compression strength to concrete, also can be shortened the production cycle to a certain extent.
Experiment effect
In order to illustrate effect of the invention, inventor determines the paste flowing degree of different experiments group under same volume, volume
Be 0.2%, according to GB T8077-2000《Methods for testing uniformity of concrete admixture》It is tested, W/C=0.29 mixes
Amount is the solid volume of folding.Commercially available polycarboxylate water-reducer, the polycarboxylate water-reducer used in control group 2 are wherein used in control group 1
Formula in addition to there is no alkyl phenol polyoxyethylene ether be formulated identical, to use in control group 3 polycarboxylate water-reducer in embodiment 3
Formula in addition to there is no cinnamic acid and octenyl succinic acid anhydride be formulated in embodiment 3 it is identical.Experimental result is shown in Table 1.Using each
In embodiment water-reducing agent be made under the same conditions measure after concrete concrete performance data it is as shown in table 2.
The net slurry mobile performance result of the different water-reducing agent types of table 1
The performance of the different concrete of table 2
It can be seen from Tables 1 and 2 from the point of view of the test result in table, due to matching for polycarboxylate water-reducer of the invention
Using alkyl phenol polyoxyethylene ether and isoamyl alcohol polyoxyethylene ether macromolecular as matrix in side, in conjunction with cinnamic acid, ascorbic acid,
A variety of acrylic acid such as octenyl succinic acid anhydride, cinnamic acid and methacrylic acid or acid anhydrides are copolymerized as monomer, because
This lacks alkyl phenol polyoxyethylene ether control group 2 using the group ratio of formula of the invention or lacks cinnamic acid and octenyl succinic
The control group 3 or commercially available polycarboxylate water-reducer of acid anhydrides have higher water-reducing rate, and have better slump holding capacity
And fluidity.80 DEG C and 45 are incorporated in by the way that various raw materials are added by several times using the embodiment 6 of the method for preparation of the invention
The mode of DEG C step heat preservation makes the concrete using embodiment 6 as water-reducing agent have lower air content than embodiment 3,
I.e. better bleed performance, on the key indexes such as compressive strength rate, shrinkage ratio also advantageously.Meanwhile passing through implementation
The polycarboxylate water-reducer of example 3 compares in the concrete of different water-binder ratios, it can be seen that polycarboxylate water-reducer of the invention is than general
Logical polycarboxylate water-reducer has higher water-reducing rate and collapsing property of guarantor is more preferable.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and embodiment shown and described herein.
Claims (6)
1. a kind of preparation method of polycarboxylate water-reducer, which is characterized in that include the following steps：
Step 1：At normal temperature, according to parts by weight, 40~60 parts of alkyl phenol polyoxyethylene ether and prenol polyoxyethylene are taken
50~80 parts of water is added after 25~35 parts of ether to be dissolved to obtain the first solution；
Step 2：According to parts by weight, by 10~15 parts of cinnamic acid, 10~15 parts of octenyl succinic acid anhydride, 3- phenyl -2- propylene
5~10 parts of acid is added 20~40 parts of water and obtains the second solution after 5~10 parts and 1 part of ascorbic acid mixing of methacrylic acid, to
Second solution is added dropwise in first solution, after obtain third solution；
Step 3：According to parts by weight, it takes 3~8 parts of isopropanol 10~20 parts of water are added and obtains the 4th solution, in the 5th solution
Including 3~8 parts of sodium peroxydisulfates and 5~10 parts of water, the third solution is heated to starting after 80 DEG C being added dropwise the described 5th molten
Liquid after 5~10min is added dropwise starts that the 4th solution is added dropwise, the 6th solution is obtained after dripping；
Step 4：6th solution is kept the temperature into 0.5~1h at 80 DEG C, is obtained after being then cooled to 45 DEG C of 1~1.5h of heat preservation
Polycarboxylate water-reducer.
2. the preparation method of polycarboxylate water-reducer as described in claim 1, which is characterized in that according to parts by weight, the step
It further include 0.5~1 part and 0.5~2 part of propylene glycol monostearate of modified rosin resin in 5th solution described in rapid three.
3. the preparation method of polycarboxylate water-reducer as described in claim 1, which is characterized in that the 4th described in the step 3
The rate of addition of solution is 1.5 times of the rate of addition of the 5th solution.
4. the preparation method of polycarboxylate water-reducer as described in claim 1, which is characterized in that by described in the step 4
It is 5.5~6.5 with the pH that sodium hydroxide adjusts the 6th solution after six solution are kept the temperature at 80 DEG C, is cooled to 45 DEG C of heat preservations 1
It is 6.5~7.5 with the pH that sodium hydroxide adjusts the 6th solution after~1.5h.
5. the preparation method of polycarboxylate water-reducer as described in claim 1, which is characterized in that by described in the step 4
Mixing speed when six solution keep the temperature 0.5~1h at 80 DEG C is 200r/min, when being then cooled to 45 DEG C of 1~1.5h of heat preservation
Mixing speed is 400r/min.
6. the preparation method of polycarboxylate water-reducer as described in claim 1, which is characterized in that the step 4 is by described the
Six solution use power to keep the temperature 0.5h for the microwave of 500W at 80 DEG C, are then cooled to 45 DEG C of microwaves for using power as 250W
Polycarboxylate water-reducer is obtained after heat preservation 0.5h.
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