CN111748067A - Method for synthesizing anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater - Google Patents
Method for synthesizing anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater Download PDFInfo
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 120
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002351 wastewater Substances 0.000 title claims abstract description 34
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 18
- 238000007710 freezing Methods 0.000 title abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000004321 preservation Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 14
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims abstract description 10
- KSVSZLXDULFGDQ-UHFFFAOYSA-M sodium;4-aminobenzenesulfonate Chemical compound [Na+].NC1=CC=C(S([O-])(=O)=O)C=C1 KSVSZLXDULFGDQ-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000009833 condensation Methods 0.000 claims abstract description 9
- 230000005494 condensation Effects 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000001502 supplementing effect Effects 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 229950000244 sulfanilic acid Drugs 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 230000002528 anti-freeze Effects 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 3
- 239000008030 superplasticizer Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 238000001308 synthesis method Methods 0.000 abstract description 3
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical class NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 10
- 125000001931 aliphatic group Chemical group 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- WPONNXIJPKZHGB-UHFFFAOYSA-N formaldehyde;sulfamic acid Chemical compound O=C.NS(O)(=O)=O WPONNXIJPKZHGB-UHFFFAOYSA-N 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 2
- YIBPLYRWHCQZEB-UHFFFAOYSA-N formaldehyde;propan-2-one Chemical class O=C.CC(C)=O YIBPLYRWHCQZEB-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 description 2
- 230000002633 protecting effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 101000802895 Dendroaspis angusticeps Fasciculin-1 Proteins 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 101000618110 Homo sapiens Sperm-associated antigen 7 Proteins 0.000 description 1
- 102100021912 Sperm-associated antigen 7 Human genes 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 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
- 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
- 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
- C04B24/226—Sulfonated naphtalene-formaldehyde condensation products
-
- 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)
- 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)
- Removal Of Specific Substances (AREA)
Abstract
The invention provides a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater, which comprises the following steps of: weighing a certain amount of acetic acid wastewater, adding the acetic acid wastewater into a reaction kettle, adding water or not, then adding sulfanilic acid or sodium sulfanilate while stirring, adding phenol when heating to 40 +/-3 ℃, continuously adding alkali when heating to 60 +/-3 ℃ while stirring, adjusting the pH value to 8.5-10, then slowly dropwise adding a formaldehyde solution, heating to raise the temperature after dropwise adding is finished, carrying out condensation and heat preservation, and supplementing water and cooling after the heat preservation is finished. The synthesis method is simple, the reaction conditions are easy to control, no three wastes are discharged, and when the prepared sulfamic acid series high-efficiency water reducing agent is applied to concrete, the antifreezing effect and the early strength effect are good, and the collapse protection effect is good.
Description
Technical Field
The invention relates to the technical field of water reducing agents, in particular to a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent by using acetic acid wastewater.
Background
The water reducing agent is used as the most additive for concrete, can reduce the water consumption in concrete mixtures, and has a good effect on improving the concrete performance of concrete. At present, a first-generation common water reducer, a second-generation high-efficiency water reducer and a third-generation high-performance water reducer are researched. The aliphatic water reducing agent (sulfonated acetone-formaldehyde condensate), the sulfamic acid high-efficiency water reducing agent (sulfamic acid-formaldehyde condensate) and the naphthalene water reducing agent (naphthalene sulfonate-formaldehyde condensate) are used as second-generation water reducing agents, and compared with third-generation polycarboxylate water reducing agents, the water reducing and collapse protecting performances of the aliphatic water reducing agent, the aliphatic water reducing agent and the sulfamic acid-based high-efficiency water reducing agent are much poorer due to the defects of the structures of the aliphatic water reducing agent, the sulfamic acid-based high-efficiency water reducing agent and the naphthalene sulfonate-formaldehyde condensate, but the naphthalene water reducing agent, the aliphatic water reducing agent.
Acetic acid is a chemical product, and is very important in chemical industrial production. It has a boiling point of 117.9 deg.C at normal pressure and a relative density of 1.0492, and is readily soluble in water, alcohols, ethers and carbon tetrachloride. Acetic acid has strong corrosivity and stabbing pain to skin, and belongs to a secondary organic acidic corrosive product. Acetic acid is used as an important reaction raw material, a solvent and the like, is widely applied to various industries, can derive hundreds of downstream products, is a key raw material or solvent of chemical products such as ethylene, acetic anhydride, cellulose acetate, acetate esters, terephthalic acid, acetate and the like, and has very wide application value.
However, in the chemical industrial production process using acetic acid, anhydrous acetic acid, or the like, a certain amount of acetic acid-containing wastewater is produced. If the waste water is directly discharged, the waste water has important influence on the environment and also causes great waste of acetic acid resources. Therefore, the recovery and the reuse of the low-concentration acetic acid wastewater have huge economic benefits and long-term environmental impact. In recent years, in order to deal with global climate change, global economic crisis and other situations, China also puts higher requirements on energy conservation and emission reduction of chemical industry than before. At present, the recycling method of the acetic acid-containing wastewater mainly comprises a rectification method, an extraction method, an adsorption method, a membrane separation method, an esterification method and the like. Among the developed physical and chemical processes, various methods have their own characteristics, and the distillation method has large energy consumption and high cost; other components are required to be added for azeotropic distillation, extractive distillation, extraction method and the like, and are recycled after separation; the main treatments of adsorption separation, membrane separation and the like are acetic acid aqueous solution with lower concentration, and are still in experimental research stage.
Therefore, no mature and complete process exists so far, which can solve the problem of recycling the acetic acid aqueous solution with the whole concentration ideally. The existing recycling treatment of acetic acid wastewater consumes more energy, easily causes waste of resources and energy sources, or possibly causes secondary environmental pollution. With the increasing awareness of people on environmental protection, the method for sustainable development, recycling economy, resource recovery and environmental protection is the main direction for acetic acid wastewater utilization in the future
Disclosure of Invention
The invention aims to provide a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater, which has the advantages of simple synthesis method, easily controlled reaction conditions and no discharge of three wastes.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater comprises the following steps: weighing a certain amount of acetic acid wastewater, adding the acetic acid wastewater into a reaction kettle, adding water or not, then adding sulfanilic acid or sodium sulfanilate while stirring, adding phenol when heating to 40 +/-3 ℃, continuously adding alkali when heating to 60 +/-3 ℃ while stirring, adjusting the pH value to 8.5-10, then slowly dropwise adding a formaldehyde solution, heating to raise the temperature after dropwise adding is finished, carrying out condensation and heat preservation, and supplementing water and cooling after the heat preservation is finished.
Preferably, the alkali is at least one of solid sodium hydroxide, sodium hydroxide aqueous solution and process waste sodium hydroxide.
Preferably, the mass ratio of the sulfanilic acid or sodium sulfanilate to the phenol is 1.55:1-1.9: 1.
Preferably, the mass ratio of the formaldehyde solution to the phenol is 1.5:1-1.8: 1;
preferably, the mass percentage concentration of the formaldehyde solution is 35-37%.
Preferably, the dripping time of the formaldehyde solution is 1.5-3.5h, and the dripping temperature is controlled to be not higher than 85 ℃ after dripping.
Preferably, the condensation heat preservation temperature is 93 +/-3 ℃, and the heat preservation time is 2-4 h.
The invention has the beneficial effects that:
1. the invention utilizes acetic acid wastewater to synthesize the antifreeze and early strength sulfamic acid high-efficiency water reducing agent, has simple synthesis method, easily controlled reaction conditions, simple production process and no discharge of three wastes, does not damage and pollute human bodies and environment, and does not cause waste of resources and energy.
2. Compared with the existing sulfonated acetone-formaldehyde condensate and sulfamic acid-formaldehyde condensate, the sulfamic acid-formaldehyde high-efficiency water reducing agent prepared by the invention has good anti-freezing effect and early-strength effect and has better collapse protection effect.
3. The method has simple treatment of the acetic acid wastewater and realizes the resource utilization of the acetic acid wastewater.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater comprises the following steps of:
weighing 100 parts of acetic acid wastewater, adding 200 parts of water into a reaction kettle, adding 160 parts of sodium sulfanilate while stirring, heating to 40 +/-3 ℃, adding 95 parts of phenol, continuously stirring while heating to 60 +/-3 ℃, adding 45 parts of sodium hydroxide solution (with the mass percentage concentration of 32%), adjusting the pH value to 9-9.5, slowly dropwise adding 160 parts of formaldehyde solution (with the mass percentage concentration of 35-37%), wherein the dropwise adding time is 2 hours, the temperature is 80 +/-3 ℃ after the dropwise adding is finished, heating to 93 +/-3 ℃, carrying out condensation and heat preservation at the temperature of 93 +/-3 ℃ for 2 hours, and supplementing 100 parts of water and cooling after the heat preservation is finished.
Example 2:
a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater comprises the following steps of:
200 parts of acetic acid wastewater is weighed and added into a reaction kettle, 100 parts of water is added, 160 parts of sulfanilic acid sodium salt is added while stirring is carried out, 95 parts of phenol is added when the temperature is heated to 40 +/-3 ℃, 65 parts of sodium hydroxide solution (with the mass percentage concentration of 32%) are added while stirring is carried out continuously and heating is carried out to 60 +/-3 ℃, the pH value is adjusted to 9-9.5, 160 parts of formaldehyde solution (with the mass percentage concentration of 35-37%) are slowly dripped, the dripping time is 2 hours, the dripping finishing temperature is 80 +/-3 ℃, the temperature is heated to 93 +/-3 ℃, the temperature is kept for 2 hours by condensation at the temperature of 93 +/-3 ℃, and 80 parts of water is added after the temperature is kept for 2 hours.
Example 3:
a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater comprises the following steps of:
adding 300 parts of acetic acid wastewater into a reaction kettle, adding 160 parts of sodium sulfanilate while stirring, beginning to add 95 parts of phenol when heating to 40 +/-3 ℃, continuing to add 85 parts of sodium hydroxide solution (with the mass percentage concentration of 32%) while stirring and heating to 60 +/-3 ℃, adjusting the pH value to 8.5-9, slowly dropwise adding 160 parts of formaldehyde solution (with the mass percentage concentration of 35-37%), wherein the dropwise adding time is 3 hours, the dropwise adding temperature is 80 +/-3 ℃, then heating to 93 +/-3 ℃, carrying out condensation and heat preservation at the temperature of 93 +/-3 ℃ for 2 hours, and supplementing 60 parts of water and cooling after the heat preservation is finished.
Example 4:
a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater comprises the following steps of:
adding 300 parts of acetic acid wastewater into a reaction kettle, adding 170 parts of sodium sulfanilate while stirring, starting to add 100 parts of phenol when heating to 40 +/-3 ℃, continuously adding 85 parts of sodium hydroxide solution (with the mass percentage concentration of 32%) when heating to 60 +/-3 ℃ while stirring, adjusting the pH value to 9-9.5, slowly adding 168 parts of formaldehyde solution (with the mass percentage concentration of 35-37%) dropwise for 3 hours, heating to 93 +/-3 ℃, keeping the temperature at 93 +/-3 ℃ for 2.5 hours, and supplementing 50 parts of water and cooling after keeping the temperature.
Example 5:
a method for synthesizing an anti-freezing early-strength sulfamic acid high-efficiency water reducing agent from acetic acid wastewater comprises the following steps of:
adding 400 parts of weighed acetic acid wastewater into a reaction kettle, adding 170 parts of sodium sulfanilate while stirring, starting to add 100 parts of phenol when heating to 40 +/-3 ℃, continuously adding 103 parts of sodium hydroxide solution (with the mass percentage concentration of 32%) when heating to 60 +/-3 ℃ while stirring, adjusting the pH value to 8.5-9, slowly adding 168 parts of formaldehyde solution (with the mass percentage concentration of 35-37%) dropwise for 3 hours, heating to 93 +/-3 ℃, keeping the temperature at 93 +/-3 ℃ for condensation and heat preservation for 2.5 hours, and cooling after the heat preservation.
According to the relevant regulations of the water reducing agent in GB 8076 plus 2008 "concrete admixture", the net slurry and the out-of-machine slump of the concrete doped with the water reducing agent prepared in the embodiment of the invention, a common aliphatic water reducing agent (represented by FAS-1) of Anhui Xin solid environmental protection technology limited company and a sulfamic acid-based high-efficiency water reducing agent (represented by SNF-1) and the ratio of the compressive strength of the concrete for 1 day, 3 days, 7 days and 28 days to the compressive strength of the reference concrete are measured, wherein the slump is 10min, 20min, 30min, 40min, 50min and 60 min. The test adopts standard cement, and the mixing amount of the water reducing agent is 0.8 percent (fold-fixed) of the weight of the cement. The specific measurement results are shown in the following table.
Table 1:
as can be seen from Table 1, the antifreezing and early strength type sulfamic acid high efficiency water reducing agent synthesized by using acetic acid wastewater by the method of the invention has good water reducing and collapse protecting effects, and the 1-day compressive strength ratio of the high efficiency water reducing agent is obviously higher than that of FSA-1 and SNF-1, thereby greatly increasing the antifreezing property of concrete.
It is noted that, herein, relational terms such as first and second, purpose-one and purpose-two, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. The method for synthesizing the antifreeze and early strength type sulfamic acid high-efficiency water reducing agent by using acetic acid wastewater is characterized by comprising the following steps of: weighing a certain amount of acetic acid wastewater, adding the acetic acid wastewater into a reaction kettle, adding water or not, then adding sulfanilic acid or sodium sulfanilate while stirring, adding phenol when heating to 40 +/-3 ℃, continuously adding alkali when heating to 60 +/-3 ℃ while stirring, adjusting the pH value to 8.5-10, then slowly dropwise adding a formaldehyde solution, heating to raise the temperature after dropwise adding is finished, carrying out condensation and heat preservation, and supplementing water and cooling after the heat preservation is finished.
2. The method for synthesizing the antifreeze early-strength sulfamic acid high-efficiency water reducer according to claim 1, wherein the alkali is at least one of solid sodium hydroxide, aqueous sodium hydroxide solution and process waste sodium hydroxide.
3. The method for synthesizing the antifreeze and early strength type sulfamic acid based superplasticizer according to claim 1, wherein the mass ratio of sulfanilic acid or sodium sulfanilate to phenol is 1.55:1-1.9: 1.
4. The method for synthesizing the antifreeze and early strength type sulfamic acid high-efficiency water reducing agent according to claim 1, wherein the mass ratio of the formaldehyde solution to the phenol is 1.5:1-1.8: 1;
5. the method for synthesizing the antifreeze early-strength sulfamic acid high-efficiency water reducing agent according to claim 4, wherein the mass percentage concentration of the formaldehyde solution is 35-37%.
6. The method for synthesizing the antifreeze early-strength sulfamic acid high-efficiency water reducing agent according to claim 1, wherein the dripping time of the formaldehyde solution is 1.5 to 3.5 hours, and the dripping temperature is controlled to be not higher than 85 ℃ after dripping.
7. The method for synthesizing the antifreeze early strength type sulfamic acid high-efficiency water reducing agent according to claim 1, wherein the condensation heat preservation temperature is 93 +/-3 ℃ and the heat preservation time is 2-4 h.
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|---|---|---|---|---|
| JPH07157350A (en) * | 1993-12-06 | 1995-06-20 | Nippon Paper Ind Co Ltd | Water reducing agent for cement |
| JPH0881248A (en) * | 1994-09-13 | 1996-03-26 | Nippon Paper Ind Co Ltd | Admixture for concrete |
| CN106277914A (en) * | 2016-08-08 | 2017-01-04 | 合肥永佳新材料科技有限公司 | A kind of anti-freezing concrete water reducer and preparation method thereof |
| CN108623767A (en) * | 2018-05-18 | 2018-10-09 | 萧县沃德化工科技有限公司 | A kind of modified amido sulfoacid series water-reducing agent of waste residue in the production process containing phenols |
| CN108864389A (en) * | 2018-07-27 | 2018-11-23 | 科之杰新材料集团有限公司 | A kind of preparation method of viscosity reduction type sulfamate water reducer |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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