CN100567197C - Utilize industrial acenaphthylene to prepare the method for efficient cement water reducing agent - Google Patents
Utilize industrial acenaphthylene to prepare the method for efficient cement water reducing agent Download PDFInfo
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- CN100567197C CN100567197C CNB2007100715235A CN200710071523A CN100567197C CN 100567197 C CN100567197 C CN 100567197C CN B2007100715235 A CNB2007100715235 A CN B2007100715235A CN 200710071523 A CN200710071523 A CN 200710071523A CN 100567197 C CN100567197 C CN 100567197C
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- reducing agent
- water reducing
- reaction
- cement water
- efficient cement
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a kind of method of utilizing industrial acenaphthylene to prepare efficient cement water reducing agent, be intended to solve in the present cement water reducing agent manufacturing problem that high quality water reducer manufacturing cost is high.It is with industrial acenaphthylene raw material, warp successively: sulfonation reaction, hydrolysis reaction, condensation reaction, neutralization reaction and make efficient cement water reducing agent.This invention is that the efficient cement water reducing agent water-reducing rate of main raw material preparation can reach 20～25% with the industrial acenaphthylene, use its concrete folding strength and ultimate compression strength of making to increase substantially, and starch degree of mobilization only and reach 230～250mm, compare with poly carboxylic acid series water reducer and aliphatic water reducing agent with performance, the production cost for preparing cement water reducing agent with industrial acenaphthylene reduces significantly.
Description
Technical field
The present invention relates to a kind of preparation method of novel concrete water reducing agent, particularly a kind of method of utilizing industrial acenaphthylene to prepare efficient cement water reducing agent.
Background technology
Cement water reducing agent claims super contracting agent again, is a kind of anion surfactant, itself not with cement generation chemical reaction, but by tensio-active agent be used for improving concrete performance, concrete is had diminishing enhanced effect significantly.Available coagulation soil water reducer mainly contains sulfonated lignin system, naphthene sulfonic acid system and poly carboxylic acid and aliphatics based water reducer.Because the prices of raw and semifnished materials are high, these high-quality cement water reducing agent manufacturing costs are very high, are unfavorable for application.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing industrial acenaphthylene to prepare efficient cement water reducing agent, to solve in the present cement water reducing agent manufacturing problem that high quality water reducer manufacturing cost is high.
In order to realize above-mentioned requirements, technical scheme of the present invention may further comprise the steps successively:
(1), sulfonation reaction: by the ratio of industrial acenaphthylene and the amount of substance of the vitriol oil is that 1: 0.8～2 the vitriol oil is added drop-wise in 80～160 ℃ the industrial acenaphthylene, is warming up to 80～160 ℃ then and carries out sulfonation, is incubated 1.5～6 hours:
(2), hydrolysis reaction: after the sulfonation reaction, be cooled to 80～140 ℃ and add the water hydrolysis, the total acidity after the hydrolysis is adjusted to 6～20%;
(3), condensation reaction: when temperature maintenance during at 50～110 ℃, be that 1: 0.6～1.6 ratio adds formaldehyde solution according to the ratio of industrial acenaphthylene and the amount of substance of formaldehyde, condensation temp is controlled at 50～115 ℃ of scopes, and is incubated 2～8 hours;
(4), neutralization reaction: add alkali, regulate pH value between 7～9, promptly obtain liquid efficient cement water reducing agent.
Advantage according to the efficient cement water reducing agent of method for preparing is: the efficient cement water reducing agent water-reducing rate that with the industrial acenaphthylene is the main raw material preparation can reach 20～25%, use its concrete folding strength and ultimate compression strength of making to increase substantially, and starch degree of mobilization only and reach 240～250mm; Compare with poly carboxylic acid series water reducer and aliphatic water reducing agent with performance, the production cost of acenaphthene water reducer reduces significantly.
Embodiment
The invention will be further described below by specific embodiment.
Embodiment 1:
(1), sulfonation reaction: in the there-necked flask of 500ml, drop into the 154g industrial acenaphthylene, be heated to 110 ℃; Drip the vitriol oil of 93g 98%, dropwised in 1 hour, 80 ℃ are incubated 4 hours, carry out sulfonation reaction, generate 2-sulfonic acid acenaphthene and 1-sulfonic acid acenaphthene.The sulfonation reaction formula is as follows:
Acenaphthene 2-sulfonic acid acenaphthene
Acenaphthene 1-sulfonic acid acenaphthene
(2), hydrolysis reaction: cooling then, add water, acidity is 7.1%, hydrolysis half an hour, 1-sulfonic acid acenaphthene is changed into 2-sulfonic acid acenaphthene.The hydrolysis reaction formula is as follows:
1-sulfonic acid acenaphthene 2-sulfonic acid acenaphthene
(3), condensation reaction: keep 70 ℃ of temperature, drip 37% formaldehyde 60g, dropwised in 1～1.5 hour, and be incubated 2.5 hours, generate sulfonic acid acenaphthene formaldehyde condensation products.The condensation reaction formula is as follows:
2-sulfonic acid acenaphthene sulfonic acid acenaphthene formaldehyde condensation products
(4), neutralization reaction: add 30% sodium hydroxide solution at last and regulate pH value to 8.0, cooling at last can obtain liquid efficient cement water reducing agent.The neutralization reaction formula is as follows:
Zhi Bei efficient cement water reducing agent is regulated proportion to 1.200 according to the method described above, and volume was at 1.6% o'clock, and flowing degree of net paste of cement reaches 245mm.Volume in the mortar is 1.8% o'clock, and its water-reducing rate can reach 23%.
Embodiment 2:
(1), sulfonation reaction: in the there-necked flask of 500ml, drop into the 154g industrial acenaphthylene, be heated to 85 ℃; Drip the vitriol oil of 198g 98%, dropwised in 1 hour, insulation is 2 hours under 90 ℃ of temperature;
(2), hydrolysis reaction: be cooled to 85 ℃ then and add water, make acidity, hydrolysis half an hour 19.2%;
(3), condensation reaction: holding temperature dropwised, and is incubated 5 hours at the formaldehyde 110g of 55 ℃ of droppings 37% in 1.5 hours;
(4), neutralization reaction: add 30% sodium hydroxide solution 100g at last, regulate pH value to 7.4 with aqua calcis again, use strainer filtering, remove throw out, liquid obtains the powdered efficient cement water reducing agent after dehydration, dry, pulverizing.
Zhi Bei powdered efficient cement water reducing agent according to the method described above, with water dissolution and regulate proportion to 1.200, volume was at 1.6% o'clock, and flowing degree of net paste of cement reaches 232mm.Volume in the mortar is 1.8% o'clock, and its water-reducing rate can reach 24.3%.
Embodiment 3:
(1), sulfonation reaction: in the there-necked flask of 500ml, drop into the 154g industrial acenaphthylene, be heated to 80 ℃; Drip the vitriol oil of 163g98%, dropwised in 1～1.5 hour, insulation is 5 hours under 150 ℃ of temperature;
(2), hydrolysis reaction: be cooled to 130 ℃ then and add water, acidity is 13.6%, hydrolysis 40 minutes;
(3), condensation reaction: holding temperature dropwised, and is incubated 4 hours at the formaldehyde 100g of 105 ℃ of droppings 37% in 2 hours;
(4), neutralization reaction: add potassium hydroxide solution at last and regulate pH value to 8, cooling at last can obtain liquid efficient cement water reducing agent.
The efficient cement water reducing agent of Zhi Bei liquid state is regulated proportion to 1.200 according to the method described above, and volume was at 1.6% o'clock, and flowing degree of net paste of cement reaches 241mm.Volume in the mortar is 1.8% o'clock, and its water-reducing rate can reach 23%.
Embodiment 4:
(1), sulfonation reaction: in the there-necked flask of 500ml, drop into the 154g industrial acenaphthylene, be heated to 110 ℃; Drip the vitriol oil of 156g98%, dropwised in 1 hour, insulation is 2 hours under 135 ℃ of temperature;
(2), hydrolysis reaction: be cooled to 120 ℃ then and add water, make acidity, hydrolysis half an hour 13%;
(3), condensation reaction: holding temperature dropwised, and is incubated 8 hours at the formaldehyde 100g of 80 ℃ of droppings 37% in 2 hours;
(4), neutralization reaction: add 30% sodium hydroxide solution at last and regulate pH value to 8.5, cooling at last can obtain liquid efficient cement water reducing agent.
The efficient cement water reducing agent of Zhi Bei liquid state is regulated proportion to 1.200 according to the method described above, and volume was at 1.6% o'clock, and flowing degree of net paste of cement reaches 253mm.Volume in the mortar is 1.8% o'clock, and its water-reducing rate can reach 25%.
Embodiment 5:
(1), sulfonation reaction: in the there-necked flask of 500ml, drop into the 154g industrial acenaphthylene, be heated to 110 ℃; Drip the vitriol oil of 156g98%, dropwised in 1～1.5 hour, insulation is 2 hours under 142 ℃ of temperature;
(2), hydrolysis reaction: be cooled to 110 ℃ then and add water, make acidity, hydrolysis half an hour 13.2%;
(3), condensation reaction: holding temperature dropwised, and is incubated 4 hours at the formaldehyde 100g of 105 ℃ of droppings 37% in 2 hours;
(4), neutralization reaction: add solid sodium hydroxide at last and regulate pH value to 7.5, cooling at last can obtain liquid efficient cement water reducing agent.
The efficient cement water reducing agent that this is liquid is regulated proportion to 1.200, and volume was at 1.6% o'clock, and flowing degree of net paste of cement reaches 248mm.Volume in the mortar is 1.8% o'clock, and its water-reducing rate can reach 25%.
In the various embodiments described above the used concrete parameter, utilize industrial acenaphthylene prepare in each step of efficient cement water reducing agent correlation parameter generally in following scope value comparatively desirable: in step (1) sulfonation reaction, the vitriol oil joins in 90-150 ℃ the acenaphthene, add-on is 1: 1～1.5 by the ratio of acenaphthene and the amount of substance of the vitriol oil, sulfonation temperature is controlled at 90-150 ℃, sulfonation insulation 2.5-4 hour; Used vitriol oil concentration is more than 95%.In step (2) hydrolysis reaction, the sulfonation reaction postcooling added the water hydrolysis 20-40 minute to 85-135 ℃, and adding water in the hydrolysis reaction, to regulate the hydrolysis total acidity be 8-16%.In step (3) condensation reaction, according to the ratio of industrial acenaphthylene and the amount of substance of formaldehyde is that 1: 0.8～1.4 ratio adds formaldehyde solution, and condensation temp is controlled at 65～105 ℃, and is incubated 3～7.5 hours, the viscosity that adds the water management material in the reaction process, used formaldehyde solution concentration is 37%.
Claims (8)
1, utilize industrial acenaphthylene to prepare the method for efficient cement water reducing agent, its feature comprises the following steps: successively
(1), sulfonation reaction: by the ratio of industrial acenaphthylene and the amount of substance of the vitriol oil is that 1: 0.8～2 the vitriol oil is added drop-wise in 80～160 ℃ the industrial acenaphthylene, is warming up to 80～160 ℃ then and carries out sulfonation, is incubated 1.5～6 hours:
(2), hydrolysis reaction: after the sulfonation reaction, be cooled to 80～140 ℃ and add the water hydrolysis, the total acidity after the hydrolysis is adjusted to 6～20%;
(3), condensation reaction: when temperature maintenance during at 50～110 ℃, be that 1: 0.6～1.6 ratio adds formaldehyde solution according to the ratio of industrial acenaphthylene and the amount of substance of formaldehyde, condensation temp is controlled at 50～115 ℃ of scopes, and is incubated 2～8 hours;
(4), neutralization reaction: add alkali, regulate pH value between 7～9, promptly obtain liquid efficient cement water reducing agent.
2, the method for utilizing industrial acenaphthylene to prepare efficient cement water reducing agent according to claim 1, it is characterized in that in step (1) sulfonation reaction, the vitriol oil joins in 90-150 ℃ the acenaphthene, add-on is 1: 1～1.5 by the ratio of acenaphthene and the amount of substance of the vitriol oil, sulfonation temperature is controlled at 90-150 ℃, sulfonation insulation 2.5-4 hour; Used vitriol oil concentration is more than 95%.
3, the method for utilizing industrial acenaphthylene to prepare efficient cement water reducing agent according to claim 1 and 2, it is characterized in that in step (2) hydrolysis reaction, the sulfonation reaction postcooling added the water hydrolysis 20-40 minute to 85-135 ℃, and adding water in the hydrolysis reaction, to regulate the hydrolysis total acidity be 8-16%.
4, the method for utilizing industrial acenaphthylene to prepare efficient cement water reducing agent according to claim 1 and 2, it is characterized in that in step (3) condensation reaction, according to the ratio of industrial acenaphthylene and the amount of substance of formaldehyde is that 1: 0.8～1.4 ratio adds formaldehyde solution, condensation temp is controlled at 65～105 ℃, and be incubated 3～7.5 hours, the viscosity that adds the water management material in the reaction process, used formaldehyde solution concentration is 37%.
5, the method for utilizing industrial acenaphthylene to prepare efficient cement water reducing agent according to claim 1 is characterized in that used alkali is solution or solid in step (4) neutralization reaction.
6,, it is characterized in that the alkali in the step (4) is sodium hydroxide or potassium hydroxide according to claim 1 or the 5 described methods of utilizing industrial acenaphthylene to prepare efficient cement water reducing agent.
7,, it is characterized in that the alkali in the step (4) is sodium hydroxide and calcium hydroxide according to claim 1 or the 5 described methods of utilizing industrial acenaphthylene to prepare efficient cement water reducing agent.
8, the method for utilizing industrial acenaphthylene to prepare efficient cement water reducing agent according to claim 1 is characterized in that making the powdered efficient cement water reducing agent with making liquid efficient cement water reducing agent through liquid-solid separation.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100715235A CN100567197C (en) | 2007-09-24 | 2007-09-24 | Utilize industrial acenaphthylene to prepare the method for efficient cement water reducing agent |
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| CNB2007100715235A CN100567197C (en) | 2007-09-24 | 2007-09-24 | Utilize industrial acenaphthylene to prepare the method for efficient cement water reducing agent |
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| CN101164955A CN101164955A (en) | 2008-04-23 |
| CN100567197C true CN100567197C (en) | 2009-12-09 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693263A (en) * | 2005-04-11 | 2005-11-09 | 广东粤和实业有限公司 | Concrete water-reducing agent and its production method |
| CN1715236A (en) * | 2004-07-02 | 2006-01-04 | 南京理工大学 | Method for preparing high efficient concrete water reducing agent using heavy washing oil |
| CN1884176A (en) * | 2006-07-11 | 2006-12-27 | 上海天弘化工有限公司 | Method for producing concrete anthracene-base additive by using anthracene slag |
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- 2007-09-24 CN CNB2007100715235A patent/CN100567197C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1715236A (en) * | 2004-07-02 | 2006-01-04 | 南京理工大学 | Method for preparing high efficient concrete water reducing agent using heavy washing oil |
| CN1693263A (en) * | 2005-04-11 | 2005-11-09 | 广东粤和实业有限公司 | Concrete water-reducing agent and its production method |
| CN1884176A (en) * | 2006-07-11 | 2006-12-27 | 上海天弘化工有限公司 | Method for producing concrete anthracene-base additive by using anthracene slag |
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| CN101164955A (en) | 2008-04-23 |
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Effective date of registration: 20090123 Address after: Zhejiang province Hangzhou City Xiasha village Nga Road No. 118 head lattice month post encoding: 310018 Applicant after: Hangzhou Huaguan Building Materials Co., Ltd. Address before: The town of Zhejiang County of Jiashan Province Hong Yang crossing Hongfu Road Post encoding: 314108 Applicant before: Jiashan Jinlong Chemicals Plant |
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