CN102321227A - Sulfonated-acetone condensate water reducing agent and preparation method thereof - Google Patents
Sulfonated-acetone condensate water reducing agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a sulfonated-acetone condensate water reducing agent and a preparation method thereof. The method is easy to operate, and the water reducing rate and storage stability of the sulfonated-acetone condensate water reducing agent can be increased effectively. The preparation method of the sulfonated-acetone condensate water reducing agent comprises the following steps of: (1) undergoing a sulfonation-condensation reaction: undergoing a sulfonation-condensation reaction on acetone, a first part of sulfonating agent and formaldehyde, wherein the molar ratio of the acetone to the formaldehyde to SO3<2-> provided in the first part of sulfonating agent is 1:(1.0-3.0):(0.30-0.70), and the molecular weight of a polymer is 40,000-80,000; and (2) undergoing a secondary sulfonation reaction: after the sulfonation-condensation reaction is completed, adding a second part of sulfonating agent for undergoing a secondary sulfonation reaction, wherein SO3<2-> provided in the second part of sulfonating agent accounts for 5-50 percent of the mole number of acetone added in to the step (1). Compared with commercially available products, the sulfonated-acetone condensate water reducing agent has the advantages of higher water reducing performance and higher storage stability.
Description
Technical field
The present invention relates to a kind of sulfonated acetone-formaldehyde condensation products water reducer and preparation method thereof.
Background technology
Sulfonated acetone-formaldehyde condensation products water reducer is to be raw material with acetone, formaldehyde, Sodium Pyrosulfite/S-WAT etc., and general technology is under alkaline matter catalysis, to make through oversulfonate and condensation.It has that production technique is simple, with short production cycle, the advantage of three-waste free discharge in production and the use, and it is low to have a raw materials for production cost, and water-reducing rate is high, and gain in strength is than very fast, and amount of air entrainment is low, does not have characteristics such as crystalline deposit phenomenon winter.To greatly develop the construction of facilities such as traffic, electric power, house in China's 12 planning; The concrete admixture industry will welcome spring; Under such opportunity, sulfonated acetone-formaldehyde condensation products water reducer also will face great market, therefore develop high diminishing sulfonated acetone-formaldehyde condensation products water reducer; Fully improve utilization ratio of raw materials, have good social and economic benefit.
Patent CN100357231 discloses a kind of preparation method of sulfonated acetone-formaldehyde condensation products high efficiency water reducing agent of Sodium sulfanilate modification; In traditional acetone synthesis technique, introduce Sodium sulfanilate; Sodium sulfanilate can addition formaldehyde and then is carried out copolycondensation with acetone-formaldehyde adduct; The high efficiency water reducing agent that makes not only water-reducing property has surpassed traditional sulfonated acetone-formaldehyde condensation products high efficiency water reducing agent, sulfamate series high-efficiency water-reducing agent and naphthalene water reducer; And slump-loss is little, has solved the concrete consistence temperature influence and has lost problem faster.But the prices of raw and semifnished materials of Sodium sulfanilate rise violently always in recent years, make that the material cost of the high efficiency water reducing agent that this modification scheme makes is higher, are unfavorable for it and apply.
Patent CN101508536 discloses the preparation method of a kind of modified sulphonated acetone-formaldehyde condensation products high efficiency water reducing agent; This method is a main raw material with acetone, formaldehyde and Sodium Pyrosulfite; With the azo-bis-isobutyl cyanide is promotor; Impel some that generate in the reaction process not possess the active double bond containing product generation radical polymerization of polycondensation, improved utilization ratio of raw materials; And then be promoting agent with vinylformic acid; Be actually the sulfonated acetone-formaldehyde condensation products high efficiency water reducing agent that has prepared a kind of poly carboxylic acid graft modification; Utilize promotor to improve raw-material utilization ratio; And come graft modification sulfonated acetone-formaldehyde condensation products water reducer with poly carboxylic acid, improved water-reducing rate and concrete other serviceabilitys of water reducer.But this method has used comparatively expensive azo-bis-isobutyl cyanide and the vinylformic acid of price to come the lower sulfonated acetone of modification price-formaldehyde condensation products water reducer on the one hand, has increased the material cost of water reducer; Because the polymerization activity of acrylic acid or the like promoting agent is bigger, reaction process is difficult to control on the other hand, easily implode and produce gel.
Therefore sulfonated acetone-formaldehyde condensation products high efficiency water reducing agent is needed a kind of operating procedure badly simply, does not increase the raw materials cost of water reducer, can effectively improve improving one's methods of its water-reducing rate.
Summary of the invention
The present invention provides the preparation method of a kind of sulfonated acetone-formaldehyde condensation products water reducer, and is simple to operate, and can effectively improve the water-reducing rate and the storage stability of gained sulfonated acetone-formaldehyde condensation products water reducer.
The present invention also provides the prepared sulfonated acetone of above-mentioned preparation method-formaldehyde condensation products water reducer.
Investigator of the present invention if can increase the sulfonate radical number in the polymer molecule, then helps improving the water-reducing property of water reducer through discovering in a large number in sulfonated acetone-formaldehyde condensation products water reducer synthetic.But in a traditional step sulfonation method,, can hinder the carrying out of polycondensation, make that the water reducer molecular weight is less than normal, not reach the ideal dispersing property if improve the sulphonating agent consumption.In order to overcome such contradiction; The investigator finds to use the secondary sulfonation method can effectively increase the number of adsorption group in the water reducer molecule; Do not reduce the molecular weight of water reducer molecule again; And then improved the water-reducing property of water reducer, and reduced the number of the reactive group in the finished product, help improving the storage stability of product.
The preparation method of said sulfonated acetone-formaldehyde condensation products water reducer may further comprise the steps:
(1) sulfonation-polyreaction: acetone, first part's sulphonating agent and formaldehyde generation sulfonation-polyreaction, wherein, the SO that is provided in acetone, formaldehyde and the first part's sulphonating agent
3 2-Mol ratio be 1: (1.0～3.0): (0.30～0.70), polymericular weight is between 4～80,000;
(2) secondary sulfonation reaction: after sulfonation-polyreaction finishes, add the second section sulphonating agent and carry out the secondary sulfonation reaction, the SO that is wherein provided in the second section sulphonating agent
3 2-Account for 5～50% of the middle acetone mole number that adds of step (1).
Preferably, S0 in acetone, formaldehyde and first part and the second section sulphonating agent
3 2-The mol ratio of summation be 1: (1.0～3.0): (0.40～0.80).
Preferably, in the step (1): under pH value 10～14 conditions, carry out sulfonation-polyreaction, first part's sulphonating agent is water-soluble; And to regulate pH value be 10～14, and temperature is controlled at 30～60 ℃, dropping acetone; The dropping time was controlled at 0.5～2 hour, dripped acetone and finished back insulation 0.5～2 hour, dripped formaldehyde again; The dropping time was controlled at 1～8 hour, and formaldehyde is warming up to 70～95 ℃ after dripping, and continued insulation 1～10 hour.
More preferably, also add the promotor that can in sulfonation-polyreaction, produce radical in the step (1) and participate in sulfonation-polyreaction, promotor and formaldehyde add together, and the consumption of said promotor is 0.2～4% of an acetone mole number.Said promotor is preferably one or more the arbitrary combination in Sodium Persulfate, Potassium Persulphate or the ammonium persulphate.
Preferably, step (2) is carried out under pH value 10～14 conditions, and the temperature of said secondary sulfonation reaction is 70～95 ℃; Reaction times is 1～5 hour.
Said sulphonating agent can be S-WAT, one or more kinds of arbitrary combination in sodium sulfite anhy 96 or the Sodium Pyrosulfite, and first part's sulphonating agent and second section sulphonating agent kind can be identical or different.
Preferably, the weight concentration of gained sulfonated acetone-formaldehyde condensation products water reducer was 20%-50% after the secondary sulfonation reaction finished.
The prepared sulfonated acetone of above-mentioned preparation method-formaldehyde condensation products water reducer is compared the sulfonated acetone-formaldehyde condensation products water reducer or the commercially available prod of traditional method preparation, has better water-reducing property and better storage stability.
During use, the conventional volume of high diminishing sulfonated acetone according to the invention-formaldehyde condensation products water reducer is 0.10%～1.5% of a cement weight.If addition is less than 0.10%, its dispersing property is unsafty so.If opposite addition surpasses 1.5%, then excessive interpolation proof only is waste economically, because do not bring the corresponding growth on the effect.
Certainly, high diminishing sulfonated acetone according to the invention-formaldehyde condensation products water reducer also can mix with at least a naphthalene water reducer known in the state of the art, thionamic acid based water reducer, sulfonated melamine-formaldehyde condensation products water reducer, Lignins ordinary water-reducing agent of being selected from mutually.In addition, except that known cement water reducing agent above-mentioned, wherein also can add air entrapment agent, swelling agent, retardant, hardening accelerator, tackifier, economization agent and skimmer etc. and mix use.
Embodiment
Following examples more detailed description prepare the process of high diminishing sulphonated acetone formaldehyde polycondensates water reducer according to the method for the invention; And these embodiment provide with the mode of explanation; Its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, but these embodiment do not limit the scope of the invention extremely.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
The molecular weight of all polycondensates uses aqueous gel chromatogram (GPC) to measure in the embodiment of the invention.Experiment condition is following:
Gel column: Shodex SB806+803 two root chromatogram columns series connection;
Moving phase: 0.1M NaNO
3The aqueous solution;
Moving phase speed: 1.0ml/min;
Injection: 20 μ l, 0.5% aqueous solution;
Detector: Shodex RI-71 type differential refraction detector;
Standard substance: polyoxyethylene glycol GPC standard specimen (Sigma-Aldrich, molecular weight 1010000,478000,263000,118000,44700,18600,6690,1960,628,232).
In the application implementation example of the present invention, the cement that is adopted is little wild field 52.5R.P.II cement, and sand is that fineness modulus is the medium sand of Mx=2.6, and stone is that particle diameter is the rubble of 5-20mm continuous grading.Concrete slump, water-reducing rate, air content test are carried out with reference to standard GB 8076-2008 " concrete admixture " relevant regulations.
Synthetic embodiment 1
S-WAT 75.6g (0.60mol) and water 300g are dropped in the 1L flask, open mechanical stirring, be warming up to 50 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 0.5g regulation system pH value to 12.0.Acetone 58.0g (1.0mol) is added dropwise to system in 1 hour, continues insulation 1 hour again.Sodium Persulfate 4.8g (0.02mol) is dissolved in 162.2g 37% formaldehyde solution (containing formaldehyde 2.0mol), and mixed solution at the uniform velocity was added dropwise in 4 hours in the reaction system, and dropping is warming up to 85 ℃ after finishing, and carries out sulfonation-polyreaction 4 hours.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 70,000.
After sulfonation-the polyreaction reaction finishes, add S-WAT 22.7g (0.18mol), this moment, system pH was 11.8, kept 85 ℃ and carried out the secondary sulfonation reaction 3 hours.After the secondary sulfonation reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 32.5%, be sorrel the system cool to room temperature.
Synthetic embodiment 2
Sodium Pyrosulfite 28.6g (0.15mol) and water 110g are dropped in the 500mL flask, open mechanical stirring, be warming up to 35 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 27.5g regulation system pH value to 10.0.Acetone 58.0g (1.0mol) is added dropwise to system in 0.5 hour, continues insulation 2 hours again.Potassium Persulphate 0.68g (0.0025mol) is dissolved in 89.2g 37% formaldehyde solution (containing formaldehyde 1.1mol), and mixed solution at the uniform velocity was added dropwise in 1 hour in the reaction system, and dropping is warming up to 95 ℃ after finishing, and carries out sulfonation-polyreaction 1 hour.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 55,000.
After sulfonation-the polyreaction reaction finishes, add Sodium Pyrosulfite 24.7g (0.13mol), using 30% sodium hydroxide solution 2.5g regulation system pH value is 10.0, keeps 95 ℃ and carries out the secondary sulfonation reaction 1 hour.After the secondary sulfonation reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 46.6%, be sorrel the system cool to room temperature.
Synthetic embodiment 3
Sodium sulfite anhy 96 72.8g (0.70mol) and water 370g are dropped in the 1L flask, open mechanical stirring, be warming up to 60 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 103.0g regulation system pH value to 14.0.Acetone 58.0g (1.0mol) is added dropwise to system in 2 hours, continues insulation 0.5 hour again.Ammonium persulphate 9.12g (0.04mol) is dissolved in 243.3g 37% formaldehyde solution (containing formaldehyde 3.0mol), and mixed solution at the uniform velocity was added dropwise in 8 hours in the reaction system, and dropping is warming up to 70 ℃ after finishing, and carries out sulfonation-polyreaction 10 hours.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 63,000.
After sulfonation-the polyreaction reaction finishes, add S-WAT 7.0g (0.056mol), this moment, system pH was 13.5, kept 70 ℃ and carried out the secondary sulfonation reaction 5 hours.After the secondary sulfonation reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 22.5%, be sorrel the system cool to room temperature.
Synthetic embodiment 4
S-WAT 12.6g (0.10mol), Sodium Pyrosulfite 20.9g (0.11mol) and water 150g are dropped in the 500mL flask, open mechanical stirring, be warming up to 55 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 1.0g regulation system pH value to 11.5.Acetone 58.0g (1.0mol) is added dropwise to system in 0.5 hour, continues insulation 0.5 hour again.Potassium Persulphate 2.7g (0.01mol) and ammonium persulphate 2.3g (0.01mol) are dissolved in 105.4g 37% formaldehyde solution (containing formaldehyde 1.3mol); Mixed solution at the uniform velocity was added dropwise in the reaction system in 2 hours; Be warming up to 80 ℃ after dripping end, carried out sulfonation-polyreaction 3 hours.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 75,000.
After sulfonation-the polyreaction reaction finishes, add sodium sulfite anhy 96 10.4g (0.10mol), this moment, system pH was 10.5, kept 85 ℃ and carried out the secondary sulfonation reaction 4 hours.After the secondary sulfonation reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 34.5%, be sorrel the system cool to room temperature.
Synthetic embodiment 5
Sodium Pyrosulfite 28.6g (0.15mol) and water 150g are dropped in the 500mL flask, open mechanical stirring, be warming up to 35 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 27.5g regulation system pH value to 10.0.Acetone 58.0g (1.0mol) is added dropwise to system in 0.5 hour, continues insulation 2 hours again.Potassium Persulphate 0.68g (0.0025mol) is dissolved in 121.6g 37% formaldehyde solution (containing formaldehyde 1.5mol), and mixed solution at the uniform velocity was added dropwise in 1 hour in the reaction system, and dropping is warming up to 90 ℃ after finishing, and carries out sulfonation-polyreaction 1 hour.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 53,000.
After sulfonation-the polyreaction reaction finishes, add Sodium Pyrosulfite 45.6g (0.24mol), using 30% sodium hydroxide solution 42.5g regulation system pH value is 12.0, keeps 90 ℃ and carries out the secondary sulfonation reaction 3 hours.After the secondary sulfonation reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 38.5%, be sorrel the system cool to room temperature.
Comparative Examples 1 (compare synthetic embodiment 1, do not add promotor in the Comparative Examples 1)
S-WAT 75.6g (0.60mol) and water 290g are dropped in the 1L flask, open mechanical stirring, be warming up to 50 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 0.5g regulation system pH value to 12.0.Acetone 58.0g (1.0mol) is added dropwise to system in 1 hour, continues insulation 1 hour again.37% formaldehyde solution 162.2g (containing formaldehyde 2.0mol) at the uniform velocity was added dropwise in 4 hours in the reaction system, and dropping is warming up to 85 ℃ after finishing, and carries out sulfonation-polyreaction 4 hours.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 67,000.
After sulfonation-the polyreaction reaction finishes, add S-WAT 22.7g (0.18mol), this moment, system pH was 11.8, kept 85 ℃ and carried out the secondary sulfonation reaction 3 hours.After the secondary sulfonation reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 31.3%, be sorrel the system cool to room temperature.
Comparative Examples 2 (compare synthetic embodiment 1, do not have the step of secondary sulfonation reaction in the Comparative Examples 2)
S-WAT 75.6g (0.60mol) and water 250g are dropped in the 1L flask, open mechanical stirring, be warming up to 50 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 0.5g regulation system pH value to 12.0.Acetone 58.0g (1.0mol) is added dropwise to system in 1 hour, continues insulation 1 hour again.Sodium Persulfate 4.8g (0.02mol) is dissolved in 162.2g 37% formaldehyde solution (containing formaldehyde 2.0mol), and mixed solution at the uniform velocity was added dropwise in 4 hours in the reaction system, and dropping is warming up to 85 ℃ after finishing, and carries out sulfonation-polyreaction 4 hours.After reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 32.3%, be sorrel the system cool to room temperature.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 69,000.
Comparative Examples 3 (compare synthetic embodiment 1, do not have the step of secondary sulfonation reaction in the Comparative Examples 3, but the sulfurous acid consumption increases to the total consumption among the synthetic embodiment 1)
S-WAT 98.3g (0.78mol) and water 300g are dropped in the 1L flask, open mechanical stirring, be warming up to 50 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 0.5g regulation system pH value to 12.0.Acetone 58.0g (1.0mol) is added dropwise to system in 1 hour, continues insulation 1 hour again.Sodium Persulfate 4.8g (0.02mol) is dissolved in 162.2g 37% formaldehyde solution (containing formaldehyde 2.0mol), and mixed solution at the uniform velocity was added dropwise in 4 hours in the reaction system, and dropping is warming up to 85 ℃ after finishing, and carries out sulfonation-polyreaction 4 hours.After reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 31.9%, be sorrel the system cool to room temperature.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 32,000.
Comparative Examples 4 (compare synthetic embodiment 1, both do not added promotor in the Comparative Examples 4, do not have the step of secondary sulfonation reaction again)
S-WAT 75.6g (0.60mol) and water 250g are dropped in the 1L flask, open mechanical stirring, be warming up to 50 ℃,, be incubated 0.5 hour with 30% sodium hydroxide solution 0.5g regulation system pH value to 12.0.Acetone 58.0g (1.0mol) is added dropwise to system in 1 hour, continues insulation 1 hour again.37% formaldehyde solution 162.2g (containing formaldehyde 2.0mol) at the uniform velocity was added dropwise in 4 hours in the reaction system, and dropping is warming up to 85 ℃ after finishing, and carries out sulfonation-condensation reaction 4 hours.After reaction finishes,, make weight concentration and be sulfonated acetone-formaldehyde condensation products water reducer aqueous solution of 31.8%, be sorrel the system cool to room temperature.Aqueous gel chromatographic determination polycondensate weight-average molecular weight is 66,000.
The application implementation example
Carried out the mensuration of water-reducing rate and air content with reference to standard GB 8076-2008 " concrete admixture " relevant regulations, the volume of each embodiment is 0.4%, and it is 21 ± 1cm that the adjustment water consumption makes the initial slump of fresh concrete, and experimental result is seen table 1.
The concrete performance evaluation table of table 1
Can find out from concrete performance data; Sulfonated acetone-formaldehyde condensation products the water reducer of the inventive method preparation compares commercially available sulfonated acetone formaldehyde condensation products water reducer mutually and naphthalene water reducer has higher water-reducing rate; And do not increase concrete air content, do not accelerate the loss of concrete slump yet.Can also find out that from the concrete data of Comparative Examples in a traditional step sulfonation method, increase sulphonating agent consumption (Comparative Examples 2 and 3), the diminishing of water reducer does not only improve, and has descended on the contrary.And the adding of promotor and secondary sulfonation reaction all have certain help to the raising (Comparative Examples 1,2 and 4) of water reducer water-reducing rate, and wherein the secondary sulfonation reaction is more obvious to the raising effect of water reducer water-reducing rate.
In order to investigate the storage stability of sulfonated acetone provided by the present invention-formaldehyde condensation products water reducer product; The present invention has carried out the evaluation of water-reducing rate to 6 months water reducer sample of storage under differing temps respectively; The water reducer volume is 0.4%; It is 21 ± 1cm that the adjustment water consumption makes the initial slump of fresh concrete, and concrete experimental result is seen table 2.
Table 2 storage stability
Storage stability data by in the last table can be found out; The sulfonated acetone formaldehyde condensation products water reducer that adopts the present invention to provide the secondary sulfonation method to make all has storage stability preferably, and it is relatively poor to use a traditional sulfonation method to make the storage stability of sulfonated acetone formaldehyde condensation products water reducer.
Claims (9)
1. the preparation method of sulfonated acetone-formaldehyde condensation products water reducer is characterized in that may further comprise the steps:
(1) sulfonation-polyreaction: acetone, first part's sulphonating agent and formaldehyde generation sulfonation-polyreaction, wherein, the SO that acetone, formaldehyde and first part's sulphonating agent provide
3 2-Mol ratio be 1: (1.0～3.0): (0.30～0.70), polymericular weight is between 4～80,000;
(2) secondary sulfonation reaction: after sulfonation-polyreaction finishes, add the second section sulphonating agent and carry out the secondary sulfonation reaction, wherein the SO that provides of second section sulphonating agent
3 2-Be 5～50% of the middle acetone mole number that adds of step (1).
2. the preparation method of sulfonated acetone as claimed in claim 1-formaldehyde condensation products water reducer is characterized in that the SO that acetone, formaldehyde and first part and second section sulphonating agent provide
3 2-The mol ratio of summation be 1: (1.0～3.0): (0.40～0.80).
3. according to claim 1 or claim 2 the preparation method of sulfonated acetone-formaldehyde condensation products water reducer is characterized in that in the step (1): under pH value 10～14 conditions, carry out sulfonation-polyreaction, and first part's sulphonating agent is water-soluble; And to regulate pH value be 10～14, and temperature is controlled at 30～60 ℃, dropping acetone; The dropping time was controlled at 0.5～2 hour; Drip acetone and finish back insulation 0.5～2 hour, drip formaldehyde again, the dropping time was controlled at 1～8 hour; Formaldehyde is warming up to 70～95 ℃ after dripping, and continues insulation 1～10 hour.
4. the preparation method of sulfonated acetone as claimed in claim 3-formaldehyde condensation products water reducer; It is characterized in that also adding in the step (1) promotor that can in sulfonation-polyreaction, produce radical and participate in sulfonation-polyreaction; Promotor and formaldehyde add together, and the consumption of said promotor is 0.2～4% of an acetone mole number.
5. the preparation method of sulfonated acetone as claimed in claim 4-formaldehyde condensation products water reducer is characterized in that said promotor is one or more the arbitrary combination in Sodium Persulfate, Potassium Persulphate or the ammonium persulphate.
6. like the preparation method of each described sulfonated acetone-formaldehyde condensation products water reducer among the claim 1-5, it is characterized in that step (2) carries out under pH value 10～14 conditions, the temperature of said secondary sulfonation reaction is 70～95 ℃; Reaction times is 1～5 hour.
7. like the preparation method of each described sulfonated acetone-formaldehyde condensation products water reducer among the claim 1-6; It is characterized in that said sulphonating agent is a S-WAT; One or more kinds of arbitrary combination in sodium sulfite anhy 96 or the Sodium Pyrosulfite, first part's sulphonating agent and second section sulphonating agent kind are identical or different.
8. like the preparation method of each described sulfonated acetone-formaldehyde condensation products water reducer among the claim 1-6, it is characterized in that the weight concentration of secondary sulfonation reaction end back gained sulfonated acetone-formaldehyde condensation products water reducer is 20%-50%.
9. the prepared sulfonated acetone of each said preparation method-formaldehyde condensation products water reducer among the claim 1-8.
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| CN102701636A (en) * | 2012-06-14 | 2012-10-03 | 吉林中路新材料有限责任公司 | Water conservancy dike, dyke soil curing agent and preparation method thereof |
| CN102701636B (en) * | 2012-06-14 | 2013-11-06 | 吉林中路新材料有限责任公司 | Water conservancy dike, dyke soil curing agent and preparation method thereof |
| CN105037670A (en) * | 2015-01-14 | 2015-11-11 | 江苏苏博特新材料股份有限公司 | High-effective water reducing agent and preparation method thereof |
| CN105037670B (en) * | 2015-01-14 | 2017-04-12 | 江苏苏博特新材料股份有限公司 | High-effective water reducing agent and preparation method thereof |
| CN105482825A (en) * | 2015-11-26 | 2016-04-13 | 河海大学 | Multifunctional soil modifier and preparation method thereof |
| 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 |
| CN108503258A (en) * | 2017-02-25 | 2018-09-07 | 北京丰乐宝科技有限公司 | A kind of cement grinding aid and its application |
| CN111087190A (en) * | 2019-12-21 | 2020-05-01 | 浙江吉盛化学建材有限公司 | Aliphatic water reducer prepared from lignosulfonate wastewater and synthesis process thereof |
| CN111848890A (en) * | 2020-06-11 | 2020-10-30 | 安徽鑫固环保股份有限公司 | Resource utilization method of 3-methyl-2-nitrobenzoic acid wastewater |
| CN112374786A (en) * | 2020-08-26 | 2021-02-19 | 安徽鑫固环保股份有限公司 | Resource utilization method of salicylic acid production wastewater |
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| CN102321227B (en) | 2012-11-21 |
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