CN108864389A - A kind of preparation method of viscosity reduction type sulfamate water reducer - Google Patents
A kind of preparation method of viscosity reduction type sulfamate water reducer Download PDFInfo
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- CN108864389A CN108864389A CN201810851262.7A CN201810851262A CN108864389A CN 108864389 A CN108864389 A CN 108864389A CN 201810851262 A CN201810851262 A CN 201810851262A CN 108864389 A CN108864389 A CN 108864389A
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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
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a kind of preparation methods of viscosity reduction type sulfamate water reducer, include the following steps：(1) p-aminobenzene sulfonic acid, phenolic compound, thinner and water are added in reaction kettle, heat up stirring and dissolving, then proceedes to be warming up to no more than 80 DEG C, start that condensing agent is slowly added dropwise, in dripping off in 2h, while maintaining the temperature at 80~90 DEG C, after being added dropwise, 1~2h is kept the temperature；(2) alkaline conditioner is added in step (1) resulting material and adjusts pH value to after 9~10, the reaction was continued；(3) reaction terminating agent and water are added into step (2) resulting material, is continuously heating to 80-90 DEG C, then keeps the temperature；(4) by step (3) resulting material be cooled to room temperature adjust pH to 7~8 to get.The present invention is by introducing thinner, the phosphate groups that high water-wet behavior is had on viscosity reduction agent molecule form one layer of stable hydration shell in particle surface energy, are conducive to the sliding of particle, the adhesive aggregation performance of clay in concrete is effectively reduced, makes concrete that there is high fluidity.
Description
Technical field
The invention belongs to build additive technical field, and in particular to a kind of preparation of viscosity reduction type sulfamate water reducer
Method.
Background technique
In recent years, it is grown rapidly with concrete technology to high-strength, green, high-performance direction, as important in concrete
The water-reducing agent of component part be also suggested it is higher, more fully require, traditional water-reducing agent has been unable to meet requirement.Traditional
Although naphthalene system and melamine superplasticizer technical maturity, due to its water-reducing rate is low, collapse damage fast and cement adaptability compared with
The reasons such as difference show obvious deficiency in terms of preparing high performance concrete, bring inconvenience to coagulation scholar construction；Polycarboxylic acids
Water-reducing agent water-reducing rate is high, it is strong to protect modeling ability, and its structure and function also have very strong designability, it is considered to be efficiently subtract
The regeneration product of aqua.However a large amount of case history and studies have shown that poly carboxylic acid series water reducer cannot solve low glue very well
The problem to become larger than bring concrete viscosity；Polycarboxylate water-reducer is influenced maximum by clay, mainly since polycarboxylic acids subtracts
Aqua molecule can be embedded in the interlayer structure of clay, consume a large amount of water-reducing agents, to influence the mobility of concrete, be increased
The cohesiveness of mixture is unfavorable for pumping and construct.
Sulfamate high-effective water-reducing agent is mainly by p-aminobenzene sulfonic acid, mononuclear aromatics derivative phenol compound and first
Aldehyde is condensed under acid or alkaline conditions, although sulfamate water reducer is a kind of high efficiency water reducing agent, but with it is other high
The effect maximum difference of water-reducing agent is that its structure has certain side chain, and suction type is also similar with polycarboxylate water-reducer, mostly tooth
The modes such as type, wire type, rather than the Planar adsorbent of other high efficiency water reducing agents, thus have water-reducing rate high, concreter can be improved
The advantages that property made and durability.For comparing polycarboxylate water-reducer, influence of the clay to sulfamate high-effective water-reducing agent is opposite
It is smaller, but there are still influences.Therefore, a kind of viscosity reduction type sulfamate water reducer is developed, existing sulfamate diminishing is solved
The problem of agent is influenced by clay, its viscosity is caused to increase, and dispersion performance reduces solves low water binder ratio concrete since viscosity increases
Cause to be difficult to the problem of constructing greatly, have great importance.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of preparation of viscosity reduction type sulfamate water reducer is provided
Method.
Technical scheme is as follows：
A kind of preparation method of viscosity reduction type sulfamate water reducer, includes the following steps：
(1) p-aminobenzene sulfonic acid, phenolic compound, thinner and water are added in reaction kettle, are warming up to 70 DEG C, stirred molten
Solution, then proceedes to be warming up to no more than 80 DEG C, starts that condensing agent is slowly added dropwise, in being dripped off in 2h, while maintaining the temperature at 80~
90 DEG C, after being added dropwise, keep the temperature 1~2h；Above-mentioned phenolic compound be phenol, bisphenol-A, bisphenol S, paracresol, metacresol and
At least one of benzenediol；The structural formula of above-mentioned thinner isIts
Middle n=5~30；Above-mentioned condensing agent is one or both of formaldehyde, acetaldehyde and furfural；
(2) be added in step (1) resulting material alkaline conditioner adjust pH value to after 9~10, the reaction was continued 1.5~
2.5h；
(3) reaction terminating agent and water are added into step (2) resulting material, is continuously heating to 80-90 DEG C, then keeps the temperature
1.5~2.5h；
(4) step (3) resulting material is cooled to room temperature, adjust pH to 7~8 to get.
In a preferred embodiment of the invention, the alkaline conditioner is sodium hydroxide and/or potassium hydroxide.
In a preferred embodiment of the invention, the reaction terminating agent be sodium hydrogensulfite, sodium pyrosulfite and
At least one of sodium sulfite.
In a preferred embodiment of the invention, in the step (3), the mass ratio of reaction terminating agent and water is 8
~12: 30.
It is further preferred that in the step (1), p-aminobenzene sulfonic acid, phenolic compound, thinner, water and condensing agent
Mass ratio be 35~60：30~70: 5~30: 200: 50~90.
Still more preferably, in the step (1), p-aminobenzene sulfonic acid, phenolic compound, thinner, water and condensation
The mass ratio of agent is 35~55: 30~67: 6~28: 200: 52~85.
Still further preferably, in the step (1), p-aminobenzene sulfonic acid, phenolic compound, thinner, water and condensation
The mass ratio of agent is 40~55: 35~67: 6~25: 200: 52~80.
The beneficial effects of the invention are as follows：
1, the present invention is added and the polynary polycondensation shapes such as phenolic compound, condensing agent and p-aminobenzene sulfonic acid by introducing thinner
At the network molecular structure with highly branched chain, diminishing agent molecule is spatially adsorbed in cement particle surface, has concrete
Good dispersibility and dispersion holding capacity.
2, the thinner that introduces has the phosphate groups of divalent in the present invention, with high water-wet behavior, easily and moisture
Son is combined with hydrogen bond formation, can be formed one layer of stable hydration shell in particle surface energy, is conducive to the sliding of particle, be effectively reduced
The cohesiveness of concrete makes concrete have high fluidity.
3, the present invention adsorbs sulfamate using cheap sodium hydrogensulfite/sodium pyrosulfite/sodium sulfite etc.
Free formaldehyde in high performance water-reducer can prevent the continuation of polycondensation reaction, avoid water-reducing agent molecular weight excessive, lead to product
It can reduce, moreover it is possible to reduce the pollution to environment.
4, simple production process of the present invention, with short production cycle, reaction temperature is mild, production operation is controllable, and product quality is steady
It is fixed.
Specific embodiment
Technical solution of the present invention is further explained and described below by way of specific embodiment.
Embodiment 1
A kind of preparation method of viscosity reduction type sulfamate water reducer, includes the following steps：
(1) in parts by mass, 55 parts of p-aminobenzene sulfonic acid, 67 parts of bisphenol-As, 25 portions of thinners and 200 parts of water are added anti-
It answers in kettle, is warming up to 70 DEG C, stirring and dissolving is continuously heating to be no more than 80 DEG C, 62 parts of formaldehyde condensation agent is then slowly added dropwise,
It is dripped off in 2h, while maintaining the temperature at 80~90 DEG C, after condensing agent is added dropwise to complete, keep the temperature 1~2h；
(2) after keeping the temperature, about 20 parts of sodium hydroxide solution regulation system pH value are added to 9~10, the reaction was continued 2h；
(3) after reaction, 12 parts of sodium hydrogensulfites and 30 parts of water are added, are continuously heating to 80~90 DEG C, keep the temperature 2h；
(4) it is cooled to room temperature, regulation system pH to 7~8 getting the products.
Embodiment 2
A kind of preparation method of viscosity reduction type sulfamate water reducer, includes the following steps：
(1) in parts by mass, reaction is added in 42 parts of p-aminobenzene sulfonic acid, 35 parts of phenol, 10 portions of thinners and 200 parts of water
In kettle, 70 DEG C are warming up to, stirring and dissolving is continuously heating to be no more than 80 DEG C, 80 parts of acetaldehyde condensation agent is then slowly added dropwise, in 2h
It inside drips off, while maintaining the temperature at 80~90 DEG C, after condensing agent is added dropwise to complete, keep the temperature 1~2h；
(2) after keeping the temperature, about 15 parts of potassium hydroxide solution regulation system pH value are added to 9~10, the reaction was continued 2h；
(3) after reaction, 10 parts of sodium sulfites and 30 parts of water are added, are continuously heating to 80~90 DEG C, keep the temperature 2h；
(4) it is cooled to room temperature, regulation system pH to 7~8 getting the products.
Embodiment 3
A kind of preparation method of viscosity reduction type sulfamate water reducer, includes the following steps：
(1) in parts by mass, xylenol, 22 portions of thinners and 200 parts of water between 50 parts of p-aminobenzene sulfonic acid, 47 parts are added
In reaction kettle, 70 DEG C are warming up to, stirring and dissolving is continuously heating to be no more than 80 DEG C, (20 parts of 70 parts of condensing agents are then slowly added dropwise
Furfural, 50 parts of formaldehyde), it is dripped off in 2h, while maintaining the temperature at 80~90 DEG C, after condensing agent is added dropwise to complete, keeps the temperature 1~2h；
(2) after keeping the temperature, about 18 parts of sodium hydroxide solution regulation system pH value are added to 9~10, the reaction was continued 2h；
(3) after reaction, 8 parts of sodium pyrosulfites and 30 parts of water are added, are continuously heating to 80~90 DEG C, keep the temperature 2h；
(4) it is cooled to room temperature, regulation system pH to 7~8 getting the products.
Embodiment 4
A kind of preparation method of viscosity reduction type sulfamate water reducer, includes the following steps：
(1) in parts by mass, by 40 parts of p-aminobenzene sulfonic acid, 15 parts of bisphenol Ss, 20 parts of phenol, 6 portions of thinners and 200 parts
Water is added in reaction kettle, is warming up to 70 DEG C, and stirring and dissolving is continuously heating to be no more than 80 DEG C, 52 parts of formaldehyde are then slowly added dropwise,
It is dripped off in 2h, while maintaining the temperature at 80~90 DEG C, after condensing agent is added dropwise to complete, keep the temperature 1~2h；
(2) after keeping the temperature, about 13 parts of sodium hydroxide solution regulation system pH value are added to 9~10, the reaction was continued 2h；
(3) after reaction, 8 parts of sodium hydrogensulfites and 30 parts of water are added, are continuously heating to 80~90 DEG C, keep the temperature 2h；
(4) it is cooled to room temperature, regulation system pH to 7~8 getting the products.
Modified sulfamate water reducer obtained by embodiment 1 to embodiment 4 is tested：Examples 1 to 4 is closed
At obtained sample, compared with commercially available sulfamate water reducer ASP, using standard cement, according to GB8076~2008
《Concrete admixture》Defined method detects the water-reducing rate of viscosity reduction type sulfamate water reducer of the invention and its to newly mixing
The influence of concrete.Concrete mix is：Cement 430kg/m3, flyash 30kg/m3, miberal powder 90kg/m3, sand 700kg/m3、
Stone 1050kg/m3, water 155kg/m3.Concrete viscosity surveys flow time by inverted slump test tube to quantify, and flow time is shorter
Show that concrete viscosity is smaller, specific method is：It is suitable by adjusting water-reducing agent volume control each sample initial extension degree, then will
Slump cone is inverted, and bottom adds quickly-opened capping, fills concrete and smooth out, and is inverted slump cone and is fixed in rack
On, bottom is not preferably less than 500mm far from ground, slips off bottom cover rapidly, tests concrete flowing time, acquired results such as table with stopwatch
Shown in 1.
1 testing concrete performance result of table
As shown in Table 1, compared with commercial product, had using viscosity reduction type sulfamate water reducer prepared by the present invention and subtracted
Water rate is high, and function of slump protection is good, and mixture workability is good, and flow velocity is fast, expects the advantages that soft, when the Examples 1 to 4 emptying of falling slump
Between be significantly less than commercial product, show sulfamate water reducer prepared by the present invention, the viscosity of concrete can be effectively reduced, change
The workability of kind concrete.
Those of ordinary skill in the art it is found that when technical parameter and raw material components of the invention changes in following ranges,
It remains to access same as the previously described embodiments or similar technical effect, still belong to and protection scope of the present invention：
A kind of preparation method of viscosity reduction type sulfamate water reducer, includes the following steps：
(1) p-aminobenzene sulfonic acid, phenolic compound, thinner and water are added in reaction kettle, are warming up to 70 DEG C, stirred molten
Solution, then proceedes to be warming up to no more than 80 DEG C, starts that condensing agent is slowly added dropwise, in being dripped off in 2h, while maintaining the temperature at 80~
90 DEG C, after being added dropwise, keep the temperature 1~2h；Above-mentioned phenolic compound be phenol, bisphenol-A, bisphenol S, paracresol, metacresol and
At least one of benzenediol；The structural formula of above-mentioned thinner isIts
Middle n=5~30；Above-mentioned condensing agent is one or both of formaldehyde, acetaldehyde and furfural；
(2) be added in step (1) resulting material alkaline conditioner adjust pH value to after 9~10, the reaction was continued 1.5~
2.5h；
(3) reaction terminating agent and water are added into step (2) resulting material, is continuously heating to 80-90 DEG C, then keeps the temperature
1.5~2.5h；
(4) step (3) resulting material is cooled to room temperature, adjust pH to 7~8 to get.
The alkaline conditioner is sodium hydroxide and/or potassium hydroxide.The reaction terminating agent is sodium hydrogensulfite, Jiao Ya
At least one of sodium sulphate and sodium sulfite.In the step (1), p-aminobenzene sulfonic acid, phenolic compound, thinner, water
And the mass ratio of condensing agent is 35~60：30~70：5~30：200：50~90, it is preferred that p-aminobenzene sulfonic acid, phenols chemical combination
Object, thinner, water and condensing agent mass ratio be 35~55: 30~67: 6~28: 200: 52~85.
The foregoing is only a preferred embodiment of the present invention, the range that the present invention that therefore, it cannot be limited according to is implemented, i.e.,
Equivalent changes and modifications made in accordance with the scope of the invention and the contents of the specification should still be within the scope of the present invention.
Claims (7)
1. a kind of preparation method of viscosity reduction type sulfamate water reducer, it is characterised in that：Include the following steps：
(1) p-aminobenzene sulfonic acid, phenolic compound, thinner and water are added in reaction kettle, are warming up to 70 DEG C, stirring and dissolving,
It then proceedes to be warming up to no more than 80 DEG C, starts that condensing agent is slowly added dropwise, in dripping off in 2h, while maintaining the temperature at 80~90
DEG C, after being added dropwise, keep the temperature 1~2h；Above-mentioned phenolic compound is phenol, bisphenol-A, bisphenol S, paracresol, metacresol and isophthalic
At least one of diphenol；The structural formula of above-mentioned thinner isWherein
N=5~30；Above-mentioned condensing agent is one or both of formaldehyde, acetaldehyde and furfural；
(2) be added in step (1) resulting material alkaline conditioner adjust pH value to after 9~10, the reaction was continued 1.5~
2.5h；
(3) reaction terminating agent and water are added into step (2) resulting material, is continuously heating to 80-90 DEG C, then keeps the temperature 1.5
~2.5h；
(4) step (3) resulting material is cooled to room temperature, adjust pH to 7~8 to get.
2. preparation method as described in claim 1, it is characterised in that：The alkaline conditioner is sodium hydroxide and/or hydrogen-oxygen
Change potassium.
3. preparation method as described in claim 1, it is characterised in that：The reaction terminating agent is sodium hydrogensulfite, burnt sulfurous
At least one of sour sodium and sodium sulfite.
4. preparation method as described in claim 1, it is characterised in that：In the step (3), the quality of reaction terminating agent and water
Than being 8~12: 30.
5. the preparation method as described in any claim in Claims 1-4, it is characterised in that：It is right in the step (1)
Aminobenzenesulfonic acid, phenolic compound, thinner, water and condensing agent mass ratio be 35~60: 30~70: 5~30: 200: 50~
90。
6. preparation method as claimed in claim 5, it is characterised in that：In the step (1), p-aminobenzene sulfonic acid, phenol generalization
The mass ratio for closing object, thinner, water and condensing agent is 35~55: 30~67: 6~28: 200: 52~85.
7. preparation method as claimed in claim 6, it is characterised in that：In the step (1), p-aminobenzene sulfonic acid, phenol generalization
The mass ratio for closing object, thinner, water and condensing agent is 40~55: 35~67: 6~25: 200: 52~80.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748067A (en) * | 2020-06-11 | 2020-10-09 | 安徽鑫固环保股份有限公司 | Method for synthesizing anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater |
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| US5879445A (en) * | 1992-10-12 | 1999-03-09 | Chryso (S.A.) | Thinners for aqueous suspensions of mineral particles and hydraulic binder pastes |
| CN106467604A (en) * | 2016-10-14 | 2017-03-01 | 科之杰新材料集团有限公司 | A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
| CN107501479A (en) * | 2017-08-16 | 2017-12-22 | 科之杰新材料集团有限公司 | A kind of preparation method of viscosity reduction type polycarboxylate water-reducer |
| CN107868187A (en) * | 2017-12-07 | 2018-04-03 | 科之杰新材料集团有限公司 | A kind of preparation method of low hydration heat polycarboxylate water-reducer |
| CN107987235A (en) * | 2017-12-07 | 2018-05-04 | 科之杰新材料集团有限公司 | A kind of preparation method of low hydration heat crack resistance type polycarboxylate water-reducer |
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2018
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5879445A (en) * | 1992-10-12 | 1999-03-09 | Chryso (S.A.) | Thinners for aqueous suspensions of mineral particles and hydraulic binder pastes |
| CN106467604A (en) * | 2016-10-14 | 2017-03-01 | 科之杰新材料集团有限公司 | A kind of viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
| CN107501479A (en) * | 2017-08-16 | 2017-12-22 | 科之杰新材料集团有限公司 | A kind of preparation method of viscosity reduction type polycarboxylate water-reducer |
| CN107868187A (en) * | 2017-12-07 | 2018-04-03 | 科之杰新材料集团有限公司 | A kind of preparation method of low hydration heat polycarboxylate water-reducer |
| CN107987235A (en) * | 2017-12-07 | 2018-05-04 | 科之杰新材料集团有限公司 | A kind of preparation method of low hydration heat crack resistance type polycarboxylate water-reducer |
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| CN111748067A (en) * | 2020-06-11 | 2020-10-09 | 安徽鑫固环保股份有限公司 | Method for synthesizing anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater |
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