CN101941811A - Novel grafted sulphamate high-efficiency water reducing agent and preparation method thereof - Google Patents

Abstract

The invention relates to a novel grafted sulphamate high-efficiency water reducing agent, which comprises the following components in percentage by mass: 10 to 18 percent of sodium sulfanilate, 4 to 6 percent of phenol, 5 to 8 percent of lignin, 7 to 12 percent of naphthalene low-concentration powder, 7 to 15 percent of formaldehyde, 0.5 to 1.3 percent of aid and 40 to 70 percent of water. The preparation method comprises the following steps of: (1) adding the sodium sulfanilate and the phenol into a reaction kettle for stirring so as to dissolve the sodium sulfanilate, adding the lignin and the naphthalene low-concentration powder into the reaction kettle, adding the aid and keeping the temperature of between 65 and 75 DEG C for 1 hour; (2) dripping the formaldehyde, finishing the dripping within 2.5 to 3 hours, raising the temperature to between 100 and 115 DEG C, reacting for 2 to 3 hours at constant temperature, stopping stirring and discharging. The provided water reducing agent has the advantages of solving the technical problem that concrete is sensitive to doping quantity and is easy to bleed and segregate by singly using the sulphamate water reducing agent, along with high water reducing ratio, high workability and obvious slump resistance.

Description

A kind of novel grafting sulfamate high-effective water-reducing agent and preparation method

Technical field

The present invention relates to the concrete water reducer, especially a kind of novel grafting sulfamate high-effective water-reducing agent and preparation method belong to building material technical field.

Background technology

Continuous development along with construction business and engineering construction, the concrete expense increases day by day, according to incompletely statistics, world's cement annual production is above 1,500,000,000 tons, amount to into concrete and should be no less than 45 billion cubic meters, about 15 billion cubic meters of the concrete amount of China wherein, the present whole world getting twice the result with half the effort from construction project, engineering structure and construction have constantly proposed new requirement to concrete performance and technology, as improve concrete intensity, wear resistance, improve the workability of fresh concrete, the slump-loss in the minimizing concrete transportation engineering etc., normal concrete has been difficult to satisfy new construction process requirement.Using admixture in concrete is effective, the easy and economic method that improves concrete strength, improves the various performances of concrete.

Water reducer is the admixture kind of consumption maximum in the concrete.The high efficiency water reducing agent water-reducing rate is greater than 12%.Can significantly improve concrete strength.High efficiency water reducing agent is divided into five big classes by its main chemical: naphthalene sulphonate formaldehyde series, melamine sulfonate and formaldehyde series, modified lignin mahogany sulfonate and derivative thereof, carboxylate salt and polycarboxylate isoreactivity polymeric superplasticizer and sulfamate water reducer.

Sulfamate high-effective water-reducing agent is late 1980s to obtain development and application research in Japan the earliest, constitutes the structure main chain by mononuclear aromatics derivative phenol and Sulphanilic Acid.Sulfamate high-effective water-reducing agent is not the bar-shaped and dentations of clamping plate on the chemical space structure, thereby its performance is better than similar naphthalene system and anthracene based water reducer.The general formula of sulfamate high-effective water-reducing agent is suc as formula shown in (I), external at material choice, synthesis technique, the physics of sulfamate high-effective water-reducing agent the application facet in the composite and concrete carried out a large amount of research.

The great advantage of sulfamate high-effective water-reducing agent is that cement adaptability is good, water-reducing rate is big, the guarantor is collapsed, and ability is strong, strength growth rate is high, this in addition admixture has certain delayed coagulation to concrete, be one of high efficiency water reducing agent of both at home and abroad tool development prospect, have development prospect preferably at home and abroad.The sulfamate high-effective water-reducing agent that uses is being produced and is being used with there being some problems at present, influence its production and application: the concrete water-retentivity is bad in application process, the segregation excreting water phenomenon is serious, even slurry hardens and water sepn, because the water reducer bleeding is big, causes the concrete water bleeding passage many, the easy crack of structure, thereby concrete durability is produced adverse influence, is exactly relatively poor to the very high cement adaptability of mineral composition tricalcium aluminate content in addition.

At above-mentioned situation, the present invention is in synthesizing amino sulfonate high efficiency water reducing agent building-up process, by a kind of polymer substance with xylogen, naphthalene system is grafted to and makes the configuration that is optimized of its molecular weight in thionamic acid water reducer synthetic, make such water reducer molecular weight size distribution trend more become reasonable, thereby solved the independent concrete that occurs with sulfamate water reducer to the responsive easily bleeding of volume, isolating technical barrier, and then concrete is effectively being improved with gain in strength under the volume, workability is effectively improved, and its function of slump protection is near the effect of polycarboxylate water-reducer.

Summary of the invention

The objective of the invention is to propose a kind of novel grafting sulfamate high-effective water-reducing agent and preparation method, thereby solved the independent concrete that occurs with sulfamate water reducer to volume responsive easily bleeding, isolating technical barrier, the water-reducing rate height, workability is good, and function of slump protection is remarkable.

The technical solution adopted in the present invention is a kind of novel grafting sulfamate high-effective water-reducing agent, it is characterized in that comprising Sodium sulfanilate, phenol, xylogen, the low dense pulvis of naphthalene system, auxiliary agent and water composition, and the mass ratio of each component is:

Sodium sulfanilate 10～18%;

Phenol 4～6%;

Xylogen 5～8%;

The low dense pulvis 7～12% of naphthalene system;

Formaldehyde 7～15%;

Auxiliary agent 0.5～1.3%;

Water 40～70%.

According to another preferred embodiment, a kind of novel grafting sulfamate high-effective water-reducing agent comprises that further the optimum quality ratio of each component is:

Sodium sulfanilate 15%;

Phenol 5%;

Xylogen 6.5%

The low dense pulvis 10.4% of naphthalene system;

Formaldehyde 10%;

Auxiliary agent 0.8%;

Water 55%.

The invention also discloses a kind of preparation method of novel grafting sulfamate high-effective water-reducing agent, may further comprise the steps:

(1) makes the Sodium sulfanilate dissolving with stirring in Sodium sulfanilate, the phenol input reactor, with xylogen, the low dense pulvis input reactor of naphthalene system, add auxiliary agent more then 65～75 ℃ of insulations 1 hour;

(2) begin to drip formaldehyde, dropwised in 2.5～3 hours, be warming up to 100～115 ℃ of isothermal reactions 2～3 hours, stop to stir discharging.

The present invention also provides a kind of application of described novel grafting sulfamate high-effective water-reducing agent, described novel grafting sulfamate high-effective water-reducing agent, and by amount of solid, volume is the 0.4-0.6% of cement quality, corresponding water-reducing rate is 30-40%.

The invention has the beneficial effects as follows:

1, the present invention is grafted to xylogen, naphthalene system in synthesizing of thionamic acid water reducer, and the molecular weight of sulfonated lignin and methoxy content are reduced, and content of phenolic hydroxyl groups raises, and hydrophobicity strengthens and force of cohesion improves, thereby has improved activity; Adding naphthalene is macromole, may enter thionamic acid water reducer main chain, also may enter side chain, thereby increase its molecular weight, overcome the thionamic acid water reducer to volume sensitivity, bleeding rate height when reducing cost, the easy isolating shortcoming of concrete makes concrete have the slump and reaches greatly that the slump is little through time loss, water retention property improves, favorable working performance, the characteristics that ultimate compression strength is high.

。2, technology of the present invention is simple, and raw material sources are extensive, and is cheap.

3, not tight to equipment requirements, less energy consumption, less investment, environmentally safe.

Embodiment

The present invention is further detailed explanation in conjunction with the preferred embodiments now.

Embodiment 1

The composition of raw materials weight ratio is:

Sodium sulfanilate 10%;

Phenol 4%;

Xylogen 5%;

The low dense pulvis 7% of naphthalene system;

Formaldehyde 7%;

Auxiliary agent 0.5%;

Water 40%.

Specific operation process is:

(1) makes the Sodium sulfanilate dissolving with stirring in Sodium sulfanilate, the phenol input reactor, then xylogen, the low dense pulvis input reactor of naphthalene system are added auxiliary agent 65 ℃ of insulations 1 hour;

(2) begin to drip formaldehyde, dropwised in 2.5 hours, be warming up to 100 ℃ of isothermal reactions 3 hours, stop to stir discharging, get novel grafting sulfamate high-effective water-reducing agent.

Embodiment 2

The composition of raw materials weight ratio is:

Sodium sulfanilate 15%;

Phenol 4.5%;

Xylogen 6%;

The low dense pulvis 9% of naphthalene system;

Formaldehyde 11%;

Auxiliary agent 0.8%;

Water 60%.

Specific operation process is:

(1) makes the Sodium sulfanilate dissolving with stirring in Sodium sulfanilate, the phenol input reactor, then xylogen, the low dense pulvis input reactor of naphthalene system are added auxiliary agent 70 ℃ of insulations 1 hour;

(2) begin to drip formaldehyde, dropwised in 2.5 hours, be warming up to 110 ℃ of isothermal reactions 2.5 hours, stop to stir discharging, get novel grafting sulfamate high-effective water-reducing agent.

Embodiment 3

The composition of raw materials weight ratio is:

Sodium sulfanilate 18%;

Phenol 6%;

Xylogen 8%;

The low dense pulvis 12% of naphthalene system;

Formaldehyde 15%;

Auxiliary agent 1.3%;

Water 70%.

Specific operation process is:

(1) makes the Sodium sulfanilate dissolving with stirring in Sodium sulfanilate, the phenol input reactor, then xylogen, the low dense pulvis input reactor of naphthalene system are added auxiliary agent 75 ℃ of insulations 1 hour;

(2) begin to drip formaldehyde, dropwised in 3 hours, be warming up to 115 ℃ of isothermal reactions 2 hours, stop to stir discharging, get novel grafting sulfamate high-effective water-reducing agent.

Embodiment 4

The composition of raw materials weight ratio is:

Sodium sulfanilate 15%;

Phenol 5%;

Xylogen 6.5%;

The low dense pulvis 10.4% of naphthalene system;

Formaldehyde 10%;

Auxiliary agent 0.8%;

Water 55%.

Specific operation process is:

(1) makes the Sodium sulfanilate dissolving with stirring in Sodium sulfanilate, the phenol input reactor, then xylogen, the low dense pulvis input reactor of naphthalene system are added auxiliary agent 75 ℃ of insulations 1 hour;

(2) begin to drip formaldehyde, dropwised in 3 hours, be warming up to 115 ℃ of isothermal reactions 2 hours, stop to stir discharging, get novel grafting sulfamate high-effective water-reducing agent.

Product performance index such as table 1 that the present invention makes:

With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and by above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification sheets, must determine its technical scope according to the claim scope.

Claims (4)

1. a novel grafting sulfamate high-effective water-reducing agent is characterized in that comprising Sodium sulfanilate, phenol, xylogen, the low dense pulvis of naphthalene system, auxiliary agent and water composition, and the mass ratio of each component is:

Sodium sulfanilate 10～18%;

Phenol 4～6%;

Xylogen 5～8%;

The low dense pulvis 7～12% of naphthalene system;

Formaldehyde 7～15%;

Auxiliary agent 0.5～1.3%;

Water 40～70%.

2. according to the described a kind of novel grafting sulfamate high-effective water-reducing agent of claim, it is characterized in that the optimum quality ratio of each component is:

Sodium sulfanilate 15%;

Phenol 5%;

Xylogen 6.5%

The low dense pulvis 10.4% of naphthalene system;

Formaldehyde 10%;

Auxiliary agent 0.8%;

Water 55%.

3. the preparation method of a novel grafting sulfamate high-effective water-reducing agent is characterized in that may further comprise the steps:

(1) makes the Sodium sulfanilate dissolving with stirring in Sodium sulfanilate, the phenol input reactor, with xylogen, the low dense pulvis input reactor of naphthalene system, add auxiliary agent more then 65～75 ℃ of insulations 1 hour;

(2) begin to drip formaldehyde, dropwised in 2.5～3 hours, be warming up to 100～115 ℃ of isothermal reactions 2～3 hours, stop to stir discharging.

4. the application of the described novel grafting sulfamate high-effective water-reducing agent of claim 1 rises and is characterised in that described novel grafting sulfamate high-effective water-reducing agent, and by amount of solid, volume is the 0.4-0.6% of cement quality, and corresponding water-reducing rate is 30-40%.