CN106830741B - A kind of poly carboxylic acid series water reducer and preparation method thereof and application method - Google Patents
A kind of poly carboxylic acid series water reducer and preparation method thereof and application method Download PDFInfo
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Abstract
The invention discloses a kind of poly carboxylic acid series water reducer and preparation method thereof and application method, the raw material of the poly carboxylic acid series water reducer includes the component of following portions by weight: 100 parts of polyethers DD-724,7~10 parts of acrylic acid, 3~7 parts of maleic anhydride, 0~2 part of methacrylic acid, 0.3~0.6 part of hydrogen peroxide, 0.5~1.0 part of initiator, 0.1~0.3 part of L-AA, 0.1~0.2 part of sodium formaldehyde sulphoxylate, 0.65~1.35 part of chain-transferring agent, 4~7 parts of pH adjusting agent and 150~170 parts of water.The cost of the poly carboxylic acid series water reducer is low, water-reducing rate is high and slump retaining is good, can be widely applied to the Important Projects such as high-speed rail, bridge, dam and the airport of various ordinary skills and different regions.The preparation method of the poly carboxylic acid series water reducer is not necessarily to heat source, and one-step polymerization, low energy consumption, reaction time is short, and production cost is low.
Description
Technical field
The present invention relates to a kind of poly carboxylic acid series water reducer and preparation method thereof and application methods.
Background technique
Cement water reducing agent is the most important auxiliary agent of concrete industry, and development course can be divided into 3 generations: first generation water-reducing agent
(the 1930s): the water-reducing agents such as lignin sulfonate and sodium abietate, stearic acid soaps.Its water-reducing rate is low, has certain
Slow setting and air-entraining effect, volume can excessively seriously affect concrete performance；Second generation water-reducing agent (the 1960s): naphthalene system,
The water-reducing agents such as melamine series, water-reducing rate is high, and not bleed, not slow setting, reinforcing effect is good, and volume is excessive to concrete performance shadow
It rings less, but the originals such as big and used naphthalene, formaldehyde, melamine of the concrete slump loss for adding this kind of water-reducing agent
Material is harmful to human body and environment；Third generation water-reducing agent (the 1980s): poly carboxylic acid series water reducer is by unsaturated fatty acid
With polyoxyethylene ether by the obtained highly -branched macromolecule dispersing agent that is graft-polymerized, compared with previous water-reducing agent, has and mix
To measure low, water-reducing rate is high, and concrete slump loss is small and does not cause obvious slow setting, and cement adaptability is good, and Harmful ingredient content is low,
The features such as proper formulation high performance concrete.
With being in full swing for infrastructure construction in china, the concrete amount that railway, highway, bridge etc. are built is significantly
Increase.Meanwhile the production of durable, weather-proof, high-strength contour performance concrete, it is increasingly dependent on high-performance polycarboxylic-acid diminishing
Agent.However, existing poly carboxylic acid series water reducer synthesis is raw materials used to be fluctuated huge, methyl alkene butyl polyoxyethylene by oil price
The cost of material such as ether, methyl allyl polyoxyethylene ether, acrylic acid and methacrylic acid it is higher (cost of material 9000~
Between 10000 yuan/ton), which greatly enhances the costs of raw material of polycarboxylate water-reducer.Meanwhile polycarboxylate water-reducer closes at present
At free radical polymerization is mostly used greatly, mostly at 40~70 DEG C, is obtained by synthesis in 4~5 hours, need to add in synthesis process
Heat not only consumes energy and also brings environmental pollution.Under the premise of guaranteeing product quality, how cost is reduced, at polycarboxylic acids diminishing
The important topic that agent faces.
Summary of the invention
Technical problem solved by the invention is to overcome the price height of existing poly carboxylic acid series water reducer, preparation process
The defect that middle reaction temperature is high, reaction time is long etc. provides a kind of poly carboxylic acid series water reducer and preparation method thereof and application method,
The poly carboxylic acid series water reducer is at low cost, water-reducing rate is high and slump retaining is good, without heat in the preparation method of the poly carboxylic acid series water reducer
Source, reaction temperature is low, and reaction time is short.
The present invention solves above-mentioned technical problem by the following technical programs.
The present invention provides a kind of poly carboxylic acid series water reducers, are made of following raw materials, and the raw material includes following weight
The component of number: DD-724100 parts of polyethers, 7~10 parts of acrylic acid, 3~7 parts of maleic anhydride, 0~2 part of methacrylic acid,
0.3~0.6 part of hydrogen peroxide, 0.5~1.0 part of initiator, 0.1~0.3 part of L-AA, sodium formaldehyde sulphoxylate 0.1~
0.2 part, 0.65~1.35 part of chain-transferring agent, 4~7 parts of pH adjusting agent and 150~170 parts of water.
Wherein, the polyethers DD-724 is Shanghai Dongda Chemical Co., Ltd.'s production, and the number of the polyethers DD-724 is equal
Molecular weight is 2800~4400, and market price is about 500 yuan/ton low compared with methyl alkene butyl polyoxyethylene ether, poly- compared with methacrylic
Ethylene oxide ether is about 200 yuan/ton low.
Wherein, the dosage of the acrylic acid is preferably 8~9 parts.
In the present invention, using cheap maleic anhydride instead of part acrylic acid and methacrylic acid, it can make
The cost of material for obtaining poly carboxylic acid series water reducer further decreases.Wherein, the dosage of the maleic anhydride is preferably 4~6
Part.
Wherein, the dosage of the methacrylic acid is preferably 0.5~1.5 part.
Wherein, the dosage of the hydrogen peroxide is preferably 0.4~0.5 part.
Wherein, the initiator is initiator commonly used in the art, preferably ammonium persulfate, sodium peroxydisulfate and mistake
One of potassium sulfate is a variety of.The initiator is more preferably 0.5~0.8 part of ammonium persulfate and 0~0.2 part of persulfuric acid
Sodium, the initiator are most preferably 0.6~0.7 part of ammonium persulfate and 0.05~0.15 part of sodium peroxydisulfate；
Wherein, the dosage of the L-AA is preferably 0.15~0.25 part.
Wherein, the dosage of the sodium formaldehyde sulphoxylate is preferably 0.12~0.18 part.
Wherein, the chain-transferring agent is chain-transferring agent commonly used in the art, preferably thioacetic acid and/or sulfydryl
Propionic acid.The chain-transferring agent is more preferably 0.6~1.0 part of thioacetic acid and 0.05~0.35 part of mercaptopropionic acid, the chain
Transfer agent is most preferably 0.7~0.9 part of thioacetic acid and 0.1~0.3 part of mercaptopropionic acid.
Wherein, the pH adjusting agent is pH adjusting agent commonly used in the art, preferably sodium hydroxide and/or hydrogen-oxygen
Change potassium.The dosage of the pH adjusting agent is preferably 5~6 parts.
Wherein, the dosage of the water is preferably 155~165 parts.
In a preferred embodiment of the present invention, the raw material includes the component of following portions by weight: polyethers DD-
724100 parts, 8~9 parts of acrylic acid, 4~6 parts of maleic anhydride, 0.5~1.5 part of methacrylic acid, hydrogen peroxide 0.4~0.5
Part, 0.6~0.7 part of ammonium persulfate, 0.05~0.15 part of sodium peroxydisulfate, 0.15~0.25 part of L-AA, formaldehyde close time sulphur
Sour hydrogen sodium 0.12~0.18,0.7~0.9 part of thioacetic acid, 0.1~0.3 part of mercaptopropionic acid, 5~6 parts of sodium hydroxide and water 155
~165 parts.
In of the invention one more preferably embodiment, the raw material is grouped as by the group of following portions by weight: polyethers DD-
724100 parts, 8~9 parts of acrylic acid, 4~6 parts of maleic anhydride, 0.5~1.5 part of methacrylic acid, hydrogen peroxide 0.4~0.5
Part, 0.6~0.7 part of ammonium persulfate, 0.05~0.15 part of sodium peroxydisulfate, 0.15~0.25 part of L-AA, formaldehyde close time sulphur
Sour hydrogen sodium 0.12~0.18,0.7~0.9 part of thioacetic acid, 0.1~0.3 part of mercaptopropionic acid, 5~6 parts of sodium hydroxide and water 155
~165 parts.
Poly carboxylic acid series water reducer of the invention is colourless to light yellow transparent liquid, the wherein concentration one of effective active composition
As be 43%~47%.
The present invention also provides the preparation methods of foregoing poly carboxylic acid series water reducer, walk by the technique of this field routine
Suddenly, the raw material in addition to the pH adjusting agent is mixed and carries out polymerization reaction, object after reacting then is adjusted with the pH adjusting agent
The pH value of material to 6.0~7.0 to get.
In a preferred embodiment of the present invention, the preparation method of the poly carboxylic acid series water reducer includes the following steps:
(1) under room temperature and stirring, solution A and solution B are added into bottom material C, carries out polymerization reaction；It is described molten
The addition opportunity of liquid B earlier than the solution A, the addition speed of the solution A be subject to 30~60min when add, the solution B
Addition speed be subject to 40~70min when add；The solution A includes the component of following parts by weight: acrylic acid 7~10
Part, 0~2 part of methacrylic acid, 3~7 parts of maleic anhydride, 0.15~0.35 part of L-AA, formaldehyde close bisulphite
0.1~0.2 part of sodium, 0.65~1.35 part of chain-transferring agent and 41~49 parts of water；The solution B includes the group of following parts by weight
Point: 0.5~1.0 part and 53~61 parts of water of initiator；The bottom material C includes the component of following parts by weight: polyethers DD-724100
Part, 0.3~0.6 part of hydrogen peroxide and 56~60 parts of water；
(2) with the pH value of the material after the pH adjusting agent telo merization of 4~7 parts by weight to 6.0~7.0 to get.
Wherein, the optimum condition of the solution A, solution B, bottom material C and each component in pH adjusting agent is all as previously described.It presses
Common sense in the field, the solution A, solution B and bottom material C are operated by mixing to uniform respectively using preceding.
In the better embodiment, the preparation method, which carries out protection without inert atmosphere, to be carried out.
In step (1), there is no particular/special requirement for the speed of the stirring, if can make the solution A, solution B with
Bottom material C is uniformly mixed.
In step (1), the method for the addition can be the method for this field routine.The mode of the addition is preferably dripped
Add.The solution A and the solution B are more preferably added drop-wise in the bottom material C from a head tank A and a head tank B respectively.
" the addition opportunity of the solution B is earlier than the solution A " refers to that solution B, earlier than solution A, does not indicate at the time of being initially added
The solution can be generally added in " solution A is added after adding solution B " after the 1~3min for being initially added into the solution B
A.Preferably, the addition speed of the solution A be subject to 40~50min when add, the addition speed of the solution B with 50~
Subject to being added when 60min.In preparation method of the invention, under the premise of guaranteeing function of slump protection, feed time substantially shortens, and adds
Enter speed to be significantly increased；And in the preparation process of existing poly carboxylic acid series water reducer, for the function of slump protection for ensuring product, add molten
Liquid A and solution B usually require cost 3~3.5 hours.
In step (1), the method and condition of the polymerization reaction can be the method for this type of polymerization of this field routine
And condition.The preferably following method and condition of the present invention: the polymerization reaction preferably carries out in polymerization reaction kettle.Preferably
Ground, after adding the solution A and solution B, the reaction was continued 0~60min；More preferably the reaction was continued 15~45min.
In step (2), by common sense in the field, feed liquid is uniformly mixed by when pH value of the material after telo merization.
The present invention also provides the application methods of the poly carboxylic acid series water reducer described in one kind comprising following step: by institute
The poly carboxylic acid series water reducer stated is mixed with cement paste, alternatively, the poly carboxylic acid series water reducer is mixed with concrete, i.e.,
It can；Wherein, the additive amount of the poly carboxylic acid series water reducer is 0.10%~0.20% of cement weight in cement paste；It is described poly-
The additive amount of carboxylic acid water reducing agent is 0.20%~0.40% of cement weight in concrete.
Wherein, the mixed method is the method for this field routine, is subject to and is uniformly mixed.
In the present invention, the room temperature be this field conventional meaning on ambient temperature, generally 10-25 DEG C.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that:
(1) cost of poly carboxylic acid series water reducer of the invention is low, water-reducing rate is high and slump retaining is good.
(2) preparation method of poly carboxylic acid series water reducer of the invention is not necessarily to heat source, and one-step polymerization, low energy consumption, reaction time
Short, production cost is low.
(3) poly carboxylic acid series water reducer of the invention, in cement paste additive amount be cement weight 0.10%~
When 0.20%, can make the cement paste initial flow degree of the ratio of mud 0.29 is 260~290mm, and fluidity growth in 1 hour is
290~320mm；When additive amount is the 0.20%~0.40% of cement weight in concrete, fresh concrete initial slump
For 210~240mm, 1 hour slump is 185~215mm.
(4) poly carboxylic acid series water reducer of the invention can be widely applied to the high-speed rail of various ordinary skills and different regions, bridge
The Important Projects such as beam, dam and airport.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
Polyethers DD-724 is purchased from: Shanghai Dongda Chemical Co., Ltd., and number-average molecular weight is 2800~4400.
In following embodiments, number used is parts by weight.
In following embodiments, ambient temperature is 20 DEG C.
Embodiment 1
A kind of preparation method of poly carboxylic acid series water reducer comprising following step:
(1) under room temperature and stirring, solution A and solution B are added dropwise into the polymerization reaction kettle for having put into bottom material C,
Carry out polymerization reaction, the time of polymerization reaction is subject to drip solution A and solution B after the reaction was continued 45min；
Wherein, the addition opportunity of solution B is earlier than solution A, the rate of addition of solution A be subject to 40min when add, solution B
Rate of addition be subject to 50min when add；Composition in solution A are as follows: acrylic acid, methacrylic acid, maleic anhydride, L-
Ascorbic acid, sodium formaldehyde sulphoxylate, thioacetic acid, mercaptopropionic acid and 41 parts of water；Composition in solution B are as follows: ammonium persulfate,
Sodium peroxydisulfate and 53 parts of water；Composition in bottom material C are as follows: number-average molecular weight is 2800 polyethers DD-724, hydrogen peroxide and 56 parts of water；
The dosage of each substance than water is shown in Table 1, and solution A, solution B and bottom material C are being bonded to uniform behaviour using preceding progress overmulling
Make；
(2) with the pH value of the material after 5.5 parts of sodium hydroxide telo merizations to 6.0 to get.
Performance measurement is carried out to obtained poly carboxylic acid series water reducer, wherein the net slurry test carried out is referring to GB/T
8077-2000 " Methods for testing uniformity of concrete admixture " standard, concrete test are " common mixed referring to GB/T50080-2002
Solidifying soil mixture method for testing performance standard ".
Through detecting, poly carboxylic acid series water reducer of the addition relative to cement weight 0.2%, can make the ratio of mud in cement paste
Reach 260mm for 0.29 cement paste initial flow degree, it is 290mm that 1 hour fluidity, which increases,.It is added in concrete opposite
It is 210mm in the initial slump of the poly carboxylic acid series water reducer of cement weight 0.4%, fresh concrete, the slump is within 1 hour
185mm。
Embodiment 2~5
According to the method for embodiment 1 and step, by preparing poly carboxylic acid series water reducer with operating parameter according to the formula in table 1.
Table 1
The performance test results of poly carboxylic acid series water reducer obtained by embodiment 2~5 are shown in Table 1.It can from table 1
Out, poly carboxylic acid series water reducer of the invention can make when additive amount is the 0.10%~0.20% of cement weight in cement paste
The cement paste initial flow degree that the ratio of mud is 0.29 is 260~290mm, and it is 290~320mm that 1 hour fluidity, which increases,；Mixed
When additive amount is the 0.20%~0.40% of cement weight in solidifying soil, fresh concrete initial slump is 210~240mm, and 1 is small
When the slump be 185~215mm.
Claims (11)
1. a kind of poly carboxylic acid series water reducer, which is characterized in that it is made of following raw materials, and the raw material includes following portions by weight
Component: it is 100 parts of polyethers DD-724,7~10 parts of acrylic acid, 3~7 parts of maleic anhydride, 0~2 part of methacrylic acid, double
0.3~0.6 part of oxygen water, 0.5~1.0 part of initiator, 0.1~0.3 part of L-AA, sodium formaldehyde sulphoxylate 0.1~0.2
Part, 0.65~1.35 part of chain-transferring agent, 4~7 parts of pH adjusting agent and 150~170 parts of water；
Wherein, the number-average molecular weight of the polyethers DD-724 is 2800~4400.
2. poly carboxylic acid series water reducer as described in claim 1, which is characterized in that the dosage of the acrylic acid is 8~9 parts；
And/or the dosage of the maleic anhydride is 4~6 parts；
And/or the dosage of the methacrylic acid is 0.5~1.5 part；
And/or the dosage of the hydrogen peroxide is 0.4~0.5 part；
And/or the initiator is one of ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate or a variety of；
And/or the dosage of the L-AA is 0.15~0.25 part；
And/or the dosage of the sodium formaldehyde sulphoxylate is 0.12~0.18 part；
And/or the chain-transferring agent is thioacetic acid and/or mercaptopropionic acid；
And/or the pH adjusting agent is sodium hydroxide and/or potassium hydroxide；
And/or the dosage of the water is 155~165 parts.
3. poly carboxylic acid series water reducer as claimed in claim 1 or 2, which is characterized in that the initiator is 0.5~0.8 part
Ammonium persulfate and 0~0.2 part of sodium peroxydisulfate；
And/or the chain-transferring agent is 0.6~1.0 part of thioacetic acid and 0.05~0.35 part of mercaptopropionic acid；
And/or the dosage of the pH adjusting agent is 5~6 parts.
4. poly carboxylic acid series water reducer as claimed in claim 3, which is characterized in that the initiator is 0.6~0.7 part described
Ammonium persulfate and 0.05~0.15 part of the sodium peroxydisulfate；
And/or the chain-transferring agent is 0.7~0.9 part of thioacetic acid and 0.1~0.3 part of mercaptopropionic acid.
5. poly carboxylic acid series water reducer as described in claim 1, which is characterized in that the raw material includes the group of following portions by weight
Point: 100 parts of polyethers DD-724,8~9 parts of acrylic acid, 4~6 parts of maleic anhydride, 0.5~1.5 part of methacrylic acid, dioxygen
0.4~0.5 part of water, 0.6~0.7 part of ammonium persulfate, 0.05~0.15 part of sodium peroxydisulfate, 0.15~0.25 part of L-AA,
Sodium formaldehyde sulphoxylate 0.12~0.18,0.7~0.9 part of thioacetic acid, 0.1~0.3 part of mercaptopropionic acid, sodium hydroxide 5~6
Part and 155~165 parts of water.
6. poly carboxylic acid series water reducer as described in claim 1, which is characterized in that the raw material by following portions by weight component
Composition: 100 parts of polyethers DD-724,8~9 parts of acrylic acid, 4~6 parts of maleic anhydride, 0.5~1.5 part of methacrylic acid, double
0.4~0.5 part of oxygen water, 0.6~0.7 part of ammonium persulfate, 0.05~0.15 part of sodium peroxydisulfate, L-AA 0.15~0.25
Part, sodium formaldehyde sulphoxylate 0.12~0.18,0.7~0.9 part of thioacetic acid, 0.1~0.3 part of mercaptopropionic acid, sodium hydroxide 5
~6 parts and 155~165 parts of water.
7. a kind of preparation method of poly carboxylic acid series water reducer as described in any one of claims 1 to 6, which is characterized in that by this
Raw material in addition to the pH adjusting agent is mixed and carries out polymerization reaction, then with the pH tune by the processing step of field routine
Save agent adjust reacting rear material pH value to 6.0~7.0 to get.
8. a kind of preparation method of poly carboxylic acid series water reducer as described in any one of claims 1 to 6, which is characterized in that it is wrapped
Include following step:
(1) under room temperature and stirring, solution A and solution B are added into bottom material C, carries out polymerization reaction；The solution B
Addition opportunity earlier than the solution A, the addition speed of the solution A be subject to 30~60min when add, the solution B
Be added speed be subject to 40~70min when add；The solution A includes the component of following parts by weight: 7~10 parts of acrylic acid,
0~2 part of methacrylic acid, 3~7 parts of maleic anhydride, 0.15~0.35 part of L-AA, sodium formaldehyde sulphoxylate
0.1~0.2 part, 0.65~1.35 part of chain-transferring agent and 41~49 parts of water；The solution B includes the component of following parts by weight:
0.5~1.0 part and 53~61 parts of water of initiator；The bottom material C includes the component of following parts by weight: polyethers DD-724 100
Part, 0.3~0.6 part of hydrogen peroxide and 56~60 parts of water；
(2) with the pH value of the material after the pH adjusting agent telo merization of 4~7 parts by weight to 6.0~7.0 to get.
9. preparation method as claimed in claim 8, which is characterized in that in step (1), the mode of the addition is to be added dropwise；
And/or in step (1), the addition speed of the solution A be subject to 40~50min when add, the addition of the solution B
Speed be subject to 50~60min when add；
And/or in step (1), after adding the solution A and solution B, the reaction was continued 0~60min.
10. preparation method as claimed in claim 8, which is characterized in that in step (1), the solution A and the solution B point
It is not added drop-wise in the bottom material C from a head tank A and a head tank B；
And/or in step (1), after adding the solution A and solution B, the reaction was continued 15~45min.
11. a kind of application method of poly carboxylic acid series water reducer as described in any one of claims 1 to 6, which is characterized in that it is wrapped
Include following step: the poly carboxylic acid series water reducer mixed with cement paste, alternatively, by the poly carboxylic acid series water reducer with
Concrete mixing；Wherein, the additive amount of the poly carboxylic acid series water reducer be cement paste in cement weight 0.10%~
0.20%；The additive amount of the poly carboxylic acid series water reducer is 0.20%~0.40% of cement weight in concrete.
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