CN105199066A - Preparation method of modified naphthalene water reducer - Google Patents

Preparation method of modified naphthalene water reducer Download PDF

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Publication number
CN105199066A
CN105199066A CN201410230687.8A CN201410230687A CN105199066A CN 105199066 A CN105199066 A CN 105199066A CN 201410230687 A CN201410230687 A CN 201410230687A CN 105199066 A CN105199066 A CN 105199066A
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naphthalene
temperature
water reducer
water
concrete
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CN201410230687.8A
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CN105199066B (en
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魏晓宏
宋波
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Sichuan Jinjiang Building Materials Technology Co Ltd
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Sichuan Jinjiang Building Materials Technology Co Ltd
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Abstract

The invention provides a preparation method of a modified naphthalene water reducer. The preparation method comprises adding naphthalene and naphthol into a reactor according to a certain ratio, heating the materials to a temperature of 130 DEG C, adding concentrated sulfuric acid into the materials at a uniform rate in 25-30min according to a weight ratio of concentrated sulfuric acid to naphthalene and naphthol of 1.1: 1, carrying out a sulfonation reaction process on the reaction system at a temperature of 159-162 DEG C for 3h, cooling the reaction product to a temperature of 120 DEG C or less, adding cold water into the product, carrying out hydrolysis, keeping acidity in a range of 27-30%, adding ethoxylated 2-naphthol into the product according to a ratio, carrying out mixing to obtain a uniform mixture, adding formaldehyde with content of 37% into the mixture in 2h, carrying out condensation at a temperature of 110-120 DEG C, then carrying out thermal insulation at a temperature of 95-105 DEG C for 2.5h, adjusting the mixture to pH of 6-9 by an alkali so that the modified naphthalene water reducer liquid is obtained, and carrying out spray drying to obtain the modified naphthalene water reducer powder. The modified naphthalene water reducer solves the problem that after mixing with concrete, the common naphthalene water reducer causes a large concrete slump loss, and improves a water-reducing rate.

Description

The preparation method of modified naphthalene series water-reducing agent
Technical field
The present invention relates to cement water reducing agent field, refer to a kind of preparation method of modified naphthalene series water-reducing agent especially.
Background technology
In prior art, cement concrete mixes primarily of cement, sand, stone, water, and for ease of construction, wherein the add-on of water is related to concrete workability and mobility, and then affects the performances such as concrete intensity and weather resistance.Water reducer is a kind of admixture with water-reducing effect, can significantly improve concrete workability and mobility, improve concrete intensity and weather resistance; Concrete workability and mobility can be improved significantly under the prerequisite not increasing unit consumption of water; Or substantially identical and under not affecting workability condition at concrete slump, reduce concrete unit consumption of water, reduce water cement ratio, save single cement consumption.Water reducer has become the five kind necessary component of concrete except cement, sand, stone, water.
After concrete-agitating, after certain hour, stir and expect retrogradation gradually, mobility is step-down gradually, is called " slump-loss "; Its reason is mainly evaporated in time due to free water in mixture, the water suction of gathering materials and cement early hydration and the result of losing.Concrete mixing and transporting car shipment distance and the time longer, owing to there is many-sided reason such as chemical reaction, water evaporates, aggregate water suction in concrete grog, free moisture content reduces, and causes concrete slump gradual loss; Concrete belt conveyor, tumbling barrel also can cause mortar to lose, and this is also the major reason causing concrete slump loss.Concrete slump loss is excessive, will bring very large difficulty, or concrete vibrating is unreal, occurs honeycomb and scale to pumping, the process such as to build.
Although the share of market of poly carboxylic acid series water reducer presents rising situation, but still exist sandstone silt content responsive, the objective problem such as volume is responsive, as the representative of s-generation water reducer, naphthalene series high-efficiency water-reducing agent to fluctuate the feature such as little containing mud with diminishing, enhancing, stable performance good with the adaptability of different varieties cement, moderate cost, sandstone, be used widely in concrete works, share of market is still up to 30% ~ 70%.But, the Slump Time losing of Large large (slump mainly refers to concrete plasticizing capacity and pumpable performance) of its concrete batching system, cause constructional difficulties (degree of mobilization of naphthalene water reducer after 2h is almost 0), and along with the further raising that high performance concrete requires the water-reducing property of high efficiency water reducing agent, dispersing property and slump retention performance, people to the modification of naphthalene water reducer and composite, the research of amido sulfoacid series and polycarboxylic acid series high efficiency water reducing agent etc. is more and more paid attention to.Individually disclose a kind of preparation method of naphthalene water reducer in Chinese patent CN1887776A, in CN1030574A, disclose a kind of an alkarylsulphonic acid naphthene sulfonic acid aldehyde condensate high efficiency water reducing agent.But existing naphthalene water reducer is difficult to combining efficient water-reducing property and good concrete is strengthened the property, little Slump Time losing of Large can also be kept simultaneously.
Summary of the invention
The present invention proposes a kind of preparation method of modified naphthalene series water-reducing agent, can provide a kind of little loss of slump, improve the modified naphthalene series water-reducing agent of water-reducing rate.
Technical scheme of the present invention is achieved in that a. by naphthalene and naphthols according to the proportioning of 9-19:1, then joins in reactor, heats;
B. when temperature is increased to 130 DEG C, in 25-30 minute, 98% vitriol oil of naphthalene and naphthols gross weight 1.1 times is at the uniform velocity added, then 159 DEG C of-162 DEG C of sulfonation reactions 3 hours;
C. when temperature of charge is down to less than 120 DEG C, add cold water hydrolysis, maintain acidity between 27-30%, the beta naphthal Soxylat A 25-7 adding naphthalene and naphthols summation 5-10% mixes;
D. the concentration adding naphthalene and naphthols summation 65-67% in 2 hours is the formaldehyde condensation of 35%-40%, period temperature control between 110-120 DEG C;
E. add after formaldehyde, temperature controls to be incubated 2.5 hours between 95-105 DEG C, namely neutralizes PH=6-9 with bases, obtains modified naphthalene series water-reducing agent liquid product;
F. liquid product, can obtain powder-like product after spray-dried.
As preferably, the bases in described step e to be concentration be 30% sodium hydroxide solution.
As preferably, the concentration of formaldehyde in described steps d is 38%.
Compared with prior art, the invention has the advantages that: the advantage that naphthalene water reducer diminishing efficiency is high can be kept; Adopt the present invention, containing a large amount of hydroxyls in water reducer, the aquation of cement can be stoped, so the function of slump protection of water reducer can be improved, make it to also have higher degree of mobilization after 2h, be convenient to transport and construction; There is higher dissemination, hydrolysis product of cement can be made even, reduce harmful hole, the intensity after 3 days of sand-cement slurry can be improved; Water reducer is used in concrete, and the degree of mobilization reduction after 2h is that more than 6%, 28 days intensity improves more than 12%, therefore, after using the present invention, can not only ensure water-reducing effect, reduce Slump Time losing of Large, effectively can also improve cement and concrete intensity; Preparation technology is simple, easy to use, effective, practical.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment: a kind of preparation method of modified naphthalene series water-reducing agent, concrete steps are:
A. by naphthalene and naphthols according to the proportioning of 9-19:1, then join in reactor, heat;
B. when temperature is increased to 130 DEG C, in 25-30 minute, 98% vitriol oil of naphthalene and naphthols gross weight 1.1 times is at the uniform velocity added, then 159 DEG C of-162 DEG C of sulfonation reactions 3 hours;
C. when temperature of charge is down to less than 120 DEG C, add cold water hydrolysis, maintain acidity between 27-30%, the beta naphthal Soxylat A 25-7 adding naphthalene and naphthols summation 5-10% mixes;
D. the concentration adding naphthalene and naphthols summation 65-67% in 2 hours is the formaldehyde condensation of 35%-40%, period temperature control between 110-120 DEG C;
E. add after formaldehyde, temperature controls to be incubated 2.5 hours between 95-105 DEG C, namely neutralizes PH=6-9 with bases, obtains modified naphthalene series water-reducing agent liquid product;
F. liquid product, can obtain powder-like product after spray-dried.
As preferably, the bases in described step e to be concentration be 30% sodium hydroxide solution.
As preferably, the concentration of formaldehyde in described steps d is 37%.
Table 1: embodiment 1 ~ embodiment 5 formulation ratio
Table 2: the degree of mobilization of naphthalene water reducer and embodiment 1 ~ embodiment 5 changes and contrasts
In order to the effect of water reducer of the present invention is described, following table provides adds in Lafarge cement by water reducer described in the water reducer of the embodiment of the present invention 1 ~ 5 and comparative example 1 ~ 2 respectively, the contrast table of cement performance.
Table 3: water reducer of the present invention and contrast water reducer add the Performance comparision after in Lafarge cement respectively to
The testing method of water-reducing rate adopts GB8076-2008.In above-mentioned test, the testing method of the slump is: with a 100mm suitable for reading, end opening 200mm, the trumpet-shaped slump bucket of high 300mm, tamping after penetration concrete, then bucket is pulled up, concrete is because of deadweight generation slump phenomenon, the height of concrete vertex after slump is deducted with bucket high (300mm), be called slump, unit is mm.
The present invention can keep the advantage that naphthalene water reducer diminishing efficiency is high; Adopt the present invention, containing a large amount of hydroxyls in water reducer, the aquation of cement can be stoped, so the function of slump protection of water reducer can be improved, make it to also have higher degree of mobilization after 2h, be convenient to transport and construction; There is higher dissemination, hydrolysis product of cement can be made even, reduce harmful hole, the intensity after the 3d of sand-cement slurry can be improved; Water reducer is used in concrete, and the degree of mobilization reduction after 2h is that more than 6%, 28 days intensity improves more than 12%, therefore, after using the present invention, can not only ensure water-reducing effect, reduce Slump Time losing of Large, effectively can also improve cement and concrete intensity; Preparation technology is simple, easy to use, effective, practical.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. a preparation method for modified naphthalene series water-reducing agent, is characterized in that: concrete steps are:
A. by naphthalene and naphthols according to the proportioning of 9-19:1, then join in reactor, heat;
B. when temperature is increased to 130 DEG C, in 25-30 minute, 98% vitriol oil of naphthalene and naphthols gross weight 1.1 times is at the uniform velocity added, then 159 DEG C of-162 DEG C of sulfonation reactions 3 hours;
C. when temperature of charge is down to less than 120 DEG C, add cold water hydrolysis, maintain acidity between 27-30%, the beta naphthal Soxylat A 25-7 adding naphthalene and naphthols summation 5-10% mixes;
D. the concentration adding naphthalene and naphthols summation 65-67% in 2 hours is the formaldehyde condensation of 35%-40%, period temperature control between 110-120 DEG C;
E. add after formaldehyde, temperature controls to be incubated 2.5 hours between 95-105 DEG C, namely neutralizes PH=6-9 with bases, obtains modified naphthalene series water-reducing agent liquid product;
F. liquid product, can obtain powder-like product after spray-dried.
2. the preparation method of modified naphthalene series water-reducing agent according to claim 1, is characterized in that: the bases in described step e to be concentration be 30% sodium hydroxide solution.
3. the preparation method of modified naphthalene series water-reducing agent according to claim 1 and 2, is characterized in that: the concentration of formaldehyde in described steps d is 38%.
CN201410230687.8A 2014-05-28 2014-05-28 The preparation method of modified naphthalene series water-reducing agent Active CN105199066B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106432661A (en) * 2016-09-18 2017-02-22 江苏苏博特新材料股份有限公司 Modified naphthalene water reducer and preparation method thereof
CN106632930A (en) * 2016-09-18 2017-05-10 江苏苏博特新材料股份有限公司 Modified polycondensation type water reducing agent, and preparation method and application thereof
CN108239248A (en) * 2016-12-23 2018-07-03 四川金江建材科技有限公司 The preparation method of modified naphthalene series water-reducing agent

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103804620A (en) * 2013-12-30 2014-05-21 广东红墙新材料股份有限公司 Naphthalene polycarboxylate slump-keeping water reducing agent and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103804620A (en) * 2013-12-30 2014-05-21 广东红墙新材料股份有限公司 Naphthalene polycarboxylate slump-keeping water reducing agent and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘尚莲: "羟基改性萘系减水剂的合成与优化", 《山东化工》 *
宋波: "羟基改性萘系高效减水剂", 《成都师专学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106432661A (en) * 2016-09-18 2017-02-22 江苏苏博特新材料股份有限公司 Modified naphthalene water reducer and preparation method thereof
CN106632930A (en) * 2016-09-18 2017-05-10 江苏苏博特新材料股份有限公司 Modified polycondensation type water reducing agent, and preparation method and application thereof
CN106432661B (en) * 2016-09-18 2019-04-02 江苏苏博特新材料股份有限公司 A kind of modified naphthalene series water-reducing agent and preparation method thereof
CN108239248A (en) * 2016-12-23 2018-07-03 四川金江建材科技有限公司 The preparation method of modified naphthalene series water-reducing agent

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