CN107778428B - A kind of aliphatic high-efficiency water reducing agent and preparation method thereof - Google Patents
A kind of aliphatic high-efficiency water reducing agent and preparation method thereof Download PDFInfo
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- CN107778428B CN107778428B CN201711084144.XA CN201711084144A CN107778428B CN 107778428 B CN107778428 B CN 107778428B CN 201711084144 A CN201711084144 A CN 201711084144A CN 107778428 B CN107778428 B CN 107778428B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 125000001931 aliphatic group Chemical group 0.000 title claims abstract description 23
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 32
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 38
- 238000006243 chemical reaction Methods 0.000 claims description 23
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 21
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 10
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000004567 concrete Substances 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 238000006482 condensation reaction Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 8
- 239000004568 cement Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
- 150000002576 ketones Chemical class 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 150000001299 aldehydes Chemical class 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 12
- 239000000498 cooling water Substances 0.000 description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- -1 hydroxypropyl Chemical group 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 150000007974 melamines Chemical class 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 3
- WBZKQQHYRPRKNJ-UHFFFAOYSA-N disulfurous acid Chemical compound OS(=O)S(O)(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000008030 superplasticizer Substances 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 239000011372 high-strength concrete Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- 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
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/0206—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with inorganic compounds
-
- 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
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/166—Macromolecular compounds comprising sulfonate or sulfate groups obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The present invention discloses a kind of aliphatic high-efficiency water reducing agent and preparation method thereof, if carrying out condensation reaction under strong basicity catalysis using aldehyde, ketone, the positions α that it is carbonylated carry out sulfomethylation and introduce sulfonic group, and control optimum mix etc., to obtain having the molecular structure of high water reducing rate and good function of slump protection, while adding cement stimulator again in the later stage, to improve the performance of concrete, the intensity of concrete is improved, and obtains the new and effective water-reducing agent haveing excellent performance.Preparation method of the present invention is reacted in lower temperature, is not necessarily to heat source, and production process equipment is simple, is produced and is stablized quickly, production capacity is big, small investment；With low price industry byproduct sodium sulfite, material cost is reduced；Using efficient tail-gas purifying recovery method and device, reaches and discharged without " three wastes ", not only improve environment, but also reduce raw materials consumption and production cost.
Description
Technical field
The present invention relates to field of fine chemical, a kind of aliphatic high-efficiency water reducing agent and preparation method thereof is related generally to.
Background technology
With the progress of building science and technology, development " high-strength high-performance concrete technology " (including " ready-mixed concrete application
The items such as technology ", " development and application super plasticizer "）It has been included in Ministry of Construction's the enforcement period of the ninth five-year plan building trade emphasis and has promoted and applied 10
New technology, this is just badly in need of developing super plasticizer（High efficiency water reducing agent）, efficient retarding and water reducing agent etc. series of products.Make at the end of the 20th century
The most high efficiency water reducing agent of dosage is naphthalene series high-efficiency water-reducing agent（Belong to aromatic series）Product, except primary raw material crude naphthalene is in short supply and price
It is high outer, it is affected chlorion to armored concrete endurance quality（1.5%~4.0%）With sodium sulphate（16%-28%）Content all compared with
It is high；Sulfate crystal, which is precipitated, when temperature is low simultaneously blocks pipeline, causes the serious concern of each side, and has formulated many limitations and arranged
It applies.For melamine analog high efficiency water reducing agent then because cost is higher, yield is less.Meanwhile Guangdong is to accounting for national 80% yield, advantages
C80 prestressed high-strength concrete piles（PHC）It has developed rapidly, but best brand of product robs the market for accounting for Guangdong 80% in the world.Cause
And find and use new raw material and new technology route, to prevent the entrance and generation of objectionable impurities, be conducive to improve China's coagulation
The durability of soil, while developing and haveing excellent performance, the less high efficiency water reducing agent of volume has become the task of top priority instead of external product.
Therefore, the existing technology needs to be improved and developed.
Invention content
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of aliphatic high-efficiency water reducing agent and its systems
Preparation Method, it is intended to solve the problems, such as that existing naphthalene series high-efficiency water-reducing agent and melamine analog high efficiency water reducing agent production cost are high.
Technical scheme is as follows：
A kind of preparation method of aliphatic high-efficiency water reducing agent, wherein include the following steps：
Formaldehyde and sodium pyrosulfite are put into, sulfonating reaction is carried out under the conditions of condensing reflux 30-40 minutes；Acetone is put into again
After maintaining the reflux for reaction at 30 DEG C ~ 50 DEG C 20-40 minutes, pre- material A is obtained；
Water and sodium sulfite are put into, stirring and dissolving is uniform, obtains B material；
Pre- material A is added dropwise in expecting to B, is warming up to 75 DEG C ~ 80 DEG C being added dropwise in 20-40 minutes and carries out condensation isothermal reaction,
Time for adding is altogether 2-3 hours, and reaction was completed；
Water dilution is added, reduces the temperature to 55 DEG C or less acid addings and neutralizes, adjusts pH value to 11-13.5, stimulator is added.
The preparation method of the aliphatic high-efficiency water reducing agent, wherein acetone, formaldehyde, sodium pyrosulfite, sodium sulfite,
Mass ratio between water is 8.5 ~ 9.5：25~29：3.5~4.5：9~10：40~50.
The preparation method of the aliphatic high-efficiency water reducing agent, wherein the stimulator is triethanolamine slag.
The preparation method of the aliphatic high-efficiency water reducing agent, wherein the input mass ratio of the stimulator is acetone：
Stimulator=8.5 ~ 9.5:0.5~1.0.
A kind of aliphatic high-efficiency water reducing agent, wherein the aliphatic high-efficiency water reducing agent is to use aliphatic as described above
The preparation method of high efficiency water reducing agent is prepared.
Advantageous effect：The preparation method of aliphatic high-efficiency water reducing agent provided by the present invention is reacted in lower temperature, is not necessarily to
Heat source, production process equipment is simple, produces and stablizes quickly, production capacity is big, small investment；With low price industry byproduct sodium sulfite, drop
Low material cost；Using efficient tail-gas purifying recovery method and device, reach and discharged without " three wastes ", not only improves environment, but also drop
Low raw materials consumption and production cost.The high efficiency water reducing agent being prepared using preparation method of the present invention is had excellent performance, and
Objectionable impurities is few, and the content of sodium sulphate is only 3.4%, and chloride ion content is only 0.09%, is greatly reduced durable to armored concrete
The influence of property.
Specific implementation mode
A kind of aliphatic high-efficiency water reducing agent of present invention offer and preparation method thereof, to make the purpose of the present invention, technical solution
And effect is clearer, clear, the present invention is described in more detail below.It should be appreciated that specific implementation described herein
Example is only used to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of preparation method of aliphatic high-efficiency water reducing agent, is a kind of quick, high without " three wastes " aliphatic
The production method of water-reducing agent is imitated, mainly carries out condensation reaction under strong basicity catalysis using aldehyde, ketone, the positions α that it is carbonylated
It carries out sulfomethylation and introduces sulfonic group, and control optimum mix etc., to obtain with high water reducing rate and well protect
The molecular structure for performance of collapsing, while adding cement stimulator to improve the strong of concrete to improve the performance of concrete again in the later stage
Degree, and obtain the new and effective water-reducing agent haveing excellent performance.Specifically, the preparation method comprises the following steps：
Formaldehyde and sodium pyrosulfite are put into, sulfonating reaction is carried out under the conditions of condensing reflux 30-40 minutes；Acetone is put into again
After maintaining the reflux for reaction at 30 DEG C ~ 50 DEG C 20-40 minutes, the pre- material of hydroxypropyl azochlorosulfonate acid sodium and formaldehyde, acetone mixture is obtained
A；
Water and sodium sulfite are put into, stirring and dissolving is uniform, obtains B material；
Pre- material A is added dropwise in expecting to B, is warming up to 75 DEG C ~ 80 DEG C being added dropwise in 20-40 minutes and carries out condensation isothermal reaction,
Time for adding is altogether 2-3 hours, and reaction was completed；
Water dilution is added, reduces the temperature to 55 DEG C or less acid addings and neutralizes, adjusts pH value to 11-13.5, stimulator is added, i.e.,
It obtains high water-reducing rate, enhancing and protects the few aliphatic high-efficiency water reducing agent of significant effect, harmful substance that collapses.
In preparation method of the present invention to be easy to get, the industrial goods of affordable（Formaldehyde, acetone, sodium pyrosulfite）With industry pair
Product sodium sulfite etc. is primary raw material, advantageously reduces the product cost of raw material.Using different from naphthalene system（Belong to aromatic series）With
The new raw material and new technology route of melamine class carry out sulfonating reaction using the pyrosulfurous acid sodium catalyst with sulfo group to carbonyl, then
With the carry out sulfomethylation of acetone, to improve its reactivity.Above-mentioned hydroxypropyl azochlorosulfonate acid sodium and formaldehyde, acetone mixture are existed again
Sodium sulfite is catalyst, is condensed under the strong alkaline condition of a certain concentration aqueous solution of formation.Later stage adds a small amount of water
Mud exciting agent（Industry byproduct triethanolamine slag）, the input mass ratio of stimulator is acetone：Stimulator=8.5 ~ 9.5:0.5~
1.0 and cement catalyst, to improve properties of product, improve concrete strength.To obtain the superior Novel fatty of performance
The high condensation product of race's hydroxy sulfonate.
Specifically, quantitative formaldehyde and pyrosulfurous acid are disposably successively direct plungeed into the pre-ization pot for being passed through cooling water
Sodium, to carbonyl into sulfonating reaction is drawn, to improve its activity；It controls again and disposably puts into quantitative third at a temperature of 30 DEG C -50 DEG C
Ketone carries out sulfomethylation under the action of certain pH value and catalyst, introduce sulfonic group control molecular weight with it is water-soluble,
To obtain hydroxypropyl azochlorosulfonate acid sodium and formaldehyde, acetone mixture, not only shorten the reaction time, but for lower step condensation reaction smoothly into
Draw and good condition is provided.
Specifically, quantitative water and sodium sulfite are put into the cooling condensation pot with Insulation, to reach preferable
Reaction density, so that hydroxypropyl azochlorosulfonate acid sodium and formaldehyde, acetone mixture is carried out condensation reaction under strongly alkaline conditions；It is anti-using it
Heat is answered, reaction temperature is made to be raised to 75 DEG C -80 DEG C from room temperature in 20-40 minutes, inventory is added dropwise by control and cooling water is big
It is small, and the measures such as supplement recycle-water, so that condensation reaction is stablized at the temperature disclosed above and quickly carry out, to prevent temperature from crossing high resin
Change or temperature to cross low reaction incomplete, be also not required to provide heat source；And condensation reaction is completed in 2-3 hours, it is with short production cycle（4-
6 hours）, production capacity it is big（Yield is criticized up to 20 tons）, reduce production cost.
Specifically, its condensation is controlled by adjusting the quality parts ratio of acetone, formaldehyde, sodium pyrosulfite and sodium sulfite
Degree and sulfonation degree protect the good macromolecular structure that collapses to obtain having high water reducing and strength-increasing effect.In preparation method of the present invention
In, better quality number proportioning is：Acetone：8.5 ~ 9.5 parts；Formaldehyde：25 ~ 29 parts；Sodium pyrosulfite：3.5 ~ 4.5 parts；Sulfurous acid
Sodium：9 ~ 10 parts；Water：40~50 parts.
In addition, the tail gas that is generated in pre-ization and condensation reaction can introduce condensing reflux, water injection absorption cleaning
Retracting device, can not only improve production operation environment and solve the difficult problem of environmental protection, and escaped in recyclable reaction process formaldehyde, third
Ketone reduces unit consumption（About 5% ~ 8%）, reduce cost.In preparation method of the present invention, recycle-water may be used and replace part water conduct
Raw materials for production further decrease production and rise this.The recycle-water is that the tail gas that will be generated in pre-ization and condensation reaction introduces
Condensing reflux, water injection absorption cleaning retracting device in the waste water that generates.
Preparation method provided by the present invention is to accumulate development for many years, production and application experience, according to cement dispersibility
Protrusion, stable structure, synthesis reliable in quality, raw material supply abundance, the principle of economical rationality, from miscellaneous producing high-molecular
It closes in object and is selected differently from naphthalene system（Belong to aromatic series）With the new process and new material of melamine class, acetone, aldehydes, pyrosulfurous acid are selected
Low price industry or byproduct sources based on sodium and sulphite etc. are preferably gone out using the strong basicity condensation process of lower temperature
The high division object of the stronger surfactant-aliphatic hydroxyl sulphonate of dispersibility（Water soluble polymer anion surface active
Agent）.To realize nothing " three wastes ", relatively low condensation temp, without the new method of heat source, the new and effective water-reducing agent of Fast back-projection algorithm.It adopts
The high efficiency water reducing agent being prepared with preparation method of the present invention is had excellent performance, in addition to having the characteristics that possessed by high efficiency water reducing agent,
Also there is the features such as good to cement adaptability, concrete flexural strength is higher, and centrifugal concrete laitance is few, it is more favorably mixed in centrifugation
Solidifying soil product is applied with other concrete works；And objectionable impurities is few, and the content of sodium sulphate is only 3.4%, chloride ion content
Only 0.09%, greatly reduce the influence to armored concrete durability.
A kind of aliphatic high-efficiency water reducing agent is also provided in the present invention, the aliphatic high-efficiency water reducing agent is using as described above
Preparation method be prepared.
Below by way of specific embodiment, the present invention will be further described.
Embodiment 1
In the pre-ization pot of logical cooling water, in the case where starting tail gas unit and system being made to form micro-vacuum state, by mass fraction
29 parts of formaldehyde is put into, then throws 3.5 parts of sodium pyrosulfite, stirring and dissolving back flow reaction about 30 minutes；8.5 parts of acetone is added, is controlled
System is for use at mixed liquor in 30 DEG C ~ 40 DEG C back flow reactions 30 minutes.
27 parts of water is thrown to logical cooling water and the condensation pot with insulating layer（25 parts of water, 2 parts of recycle-water）, then throw sodium sulfite 9
Part, it stirs evenly, obtains sodium sulfite aqueous solution.
Aforementioned mixed liquor is slowly added dropwise in sodium sulfite aqueous solution, material is made to warm naturally to 75 DEG C in 20 minutes or so
It is above to maintain to carry out condensation reaction under constant temperature counterflow condition, aforementioned mixture was finished at 3 hours or so, insulation reaction terminates, and closes
Cooling water.Inspection by sampling is qualified, can add 20 parts of dilutions of water, open cooling water temperature to 55 DEG C hereinafter, with 2 parts of acid be neutralized to PH=11 ~
13.5, then add liquid high efficiency water reducing agent of 1 part of the three ethyl alcohol slag to get solid content about 30%.Service check is carried out to product（It presses
GB8076-1997）, inspection result is as shown in table 1.
Embodiment 2
In the pre-ization pot of logical cooling water, in the case where starting tail gas unit and system being made to form micro-vacuum state, by mass fraction
25 parts of formaldehyde is put into, then throws 4.5 parts of sodium pyrosulfite, stirring and dissolving is reacted about 40 minutes；9.5 parts of acetone is added, control exists
40 ~ 50 DEG C of back flow reactions 30 minutes are for use at mixed liquor.
20.5 parts of water is thrown to logical cooling water and the condensation pot with insulating layer（18.5 parts of water, 2 parts of recycle-water）, then throw sulfurous acid
10 parts of sodium, stirs evenly, obtains sodium sulfite aqueous solution.
Aforementioned mixed liquor is slowly added dropwise in sodium sulfite aqueous solution, material is made to warm naturally to 80 DEG C in 30 minutes or so
It maintains to carry out condensation reaction under constant temperature counterflow condition, aforementioned mixture was finished at 2 hours or so, insulation reaction terminates, and closes cooling
Water.Inspection by sampling is qualified, can add 29 parts of dilutions of water, open cooling water temperature to 55 DEG C hereinafter, with 1 part of acid be neutralized to PH=11 ~
13.5, then add liquid high efficiency water reducing agent of 0.5 part of the three ethyl alcohol slag to get solid content about 30%.Service check is carried out to product（It presses
GB8076-1997）, inspection result is as shown in table 1.
Table 1
The high efficiency water reducing agent being prepared using preparation method of the present invention, excellent product performance, except with high efficiency water reducing agent
Outside possessed feature, it is good to cement adaptability also to have, and concrete flexural strength is higher, and centrifugal concrete laitance waits spies less
Point is more favorably applied in centrifugal concrete product with other concrete works.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect range.
Claims (2)
1. a kind of preparation method of aliphatic high-efficiency water reducing agent, which is characterized in that include the following steps：
Formaldehyde and sodium pyrosulfite are put into, sulfonating reaction is carried out under the conditions of condensing reflux 30-40 minutes；Acetone is put into again 30
DEG C~50 DEG C maintain the reflux for reaction 20-40 minutes after, obtain pre- material A；
Water and sodium sulfite are put into, stirring and dissolving is uniform, obtains B material；
Pre- material A is added dropwise in expecting to B, is warming up to 75 DEG C~80 DEG C being added dropwise in 20-40 minute and carries out condensation isothermal reaction, dropwise addition
Time is altogether 2-3 hours, and reaction was completed；
Water dilution is added, reduces the temperature to 55 DEG C or less acid addings and neutralizes, adjusts pH value to 11-13.5, stimulator is added；
Mass ratio between acetone, formaldehyde, sodium pyrosulfite, sodium sulfite, water is 8.5~9.5：25~29：3.5~4.5：9
~10：40~50；
The stimulator is triethanolamine slag；
The input mass ratio of the stimulator is acetone：Stimulator=8.5~9.5:0.5~1.0.
2. a kind of aliphatic high-efficiency water reducing agent, which is characterized in that the aliphatic high-efficiency water reducing agent is using such as claim 1 institute
The preparation method for the aliphatic high-efficiency water reducing agent stated is prepared.
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| CN1634794A (en) * | 2003-12-31 | 2005-07-06 | 吴霖秀 | High efficiency aliphatic sulfonate water reducing agent and method for preparing same |
| CN101186459A (en) * | 2007-12-04 | 2008-05-28 | 北京工业大学 | Method for preparing aliphatic high efficiency water reducing agent by using industrial by-product and application thereof |
| CN101624269A (en) * | 2009-08-03 | 2010-01-13 | 常州汇迪建材有限公司 | Aliphatic series high-efficiency water reducing agent and preparation method thereof |
| CN104130361A (en) * | 2014-08-13 | 2014-11-05 | 江苏苏博特新材料股份有限公司 | Preparation method of highly-sulfonated and highly-concentrated aliphatic superplasticizer |
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| CN1634794A (en) * | 2003-12-31 | 2005-07-06 | 吴霖秀 | High efficiency aliphatic sulfonate water reducing agent and method for preparing same |
| CN101186459A (en) * | 2007-12-04 | 2008-05-28 | 北京工业大学 | Method for preparing aliphatic high efficiency water reducing agent by using industrial by-product and application thereof |
| CN101624269A (en) * | 2009-08-03 | 2010-01-13 | 常州汇迪建材有限公司 | Aliphatic series high-efficiency water reducing agent and preparation method thereof |
| CN104130361A (en) * | 2014-08-13 | 2014-11-05 | 江苏苏博特新材料股份有限公司 | Preparation method of highly-sulfonated and highly-concentrated aliphatic superplasticizer |
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