CN101391876B - Dry powder mortar additive suitable for novel wall material and preparation method thereof - Google Patents
Dry powder mortar additive suitable for novel wall material and preparation method thereof Download PDFInfo
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- CN101391876B CN101391876B CN2008100299696A CN200810029969A CN101391876B CN 101391876 B CN101391876 B CN 101391876B CN 2008100299696 A CN2008100299696 A CN 2008100299696A CN 200810029969 A CN200810029969 A CN 200810029969A CN 101391876 B CN101391876 B CN 101391876B
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Classifications
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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
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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
- C04B24/18—Lignin sulfonic acid or derivatives thereof, e.g. sulfite lye
-
- 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
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/30—Condensation polymers of aldehydes or ketones
- C04B24/307—Urea-formaldehyde condensation polymers
-
- 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
Abstract
The invention discloses an environment friendly dry mortar admixture applicable to novel wall materials, and a preparation method thereof. The method comprises the steps: (1) lignosulphonate is added with water and mixed uniformly, the system pH value is adjusted to be 8.0 to 11.0, urea and formaldehyde are added, and the mixture reacts for 1 to 2 hours at the temperature of 80 to 100 DEG C; (2) the system pH value is adjusted to be 4.0 to 6.0, and the mixture reacts for 2 to 3 hours at the temperature of 80 to 100 DEG C; and (3) an oxidant is added, the mixture reacts for 1 to 2 hours at the temperature of 70 to 90 DEG C and is cooled to obtain the liquid product of the mortar admixture, and the powder product of the mortar admixture can be obtained after spray drying. The mortar admixture has simple preparation process and low production cost, is environment-friendly as the papermaking and pulping by-product, lignosulphonate, is taken as raw material, has high water reduction rate, appropriate retardation and air-entraining performance, and can cause the mortar to have good cohesiveness, anti-cracking and impermeability.
Description
Technical field
The present invention relates to a kind of environment-friendly highly efficient dry powder mortar additive that is applicable to novel wall material and preparation method thereof, belong to building material field; The recovery product sulfonated lignin of more specifically saying so with acid polishing effluent are raw material, mortar additive that is prepared from through modification and preparation method thereof.
Background technology
Utilize novel wall material instead of clay solid brick, can improve building function, promote the technical progress of construction industry, save energy is all having important meaning aspect the utilization of refuse and the environment protection.In promoting the use of novel wall material, no matter be bearing wall, or the infilled wall in the skeleton construction, wall crazing that ubiquity is serious and leakage problems have had a strong impact on construction quality and have used with normal, have also seriously restricted applying of novel wall material.Novel wall material rimose major cause is that traditional sand-cement slurry of employing or mixed mortar self shrink greatly, cohesive strength is low and mate unreasonable.
The quality of the good and bad directly influence building masonry project of building mortar performance.The tradition mortar mainly is made up of cement, sand, lime putty and water; Wherein lime putty has material impact to the quality and the workability of mortar; That such mortar shrinks is big, serviceability and water retention property are relatively poor, is prone to cause the generation of accidents resulting from poor quality of projects such as masonry mortar layer hollowing, cracking, strength degradation.On the mortar mode of production change having taken place abroad for this reason, no longer mixed and stirred with cement, sand and water scene by construction enterprises, but supplies construction enterprises to select for use by specialized factory according to the commodity dry-mix that different purposes are prefabricated into seriation.Dry-mix obtained development rapidly in China in recent years, was quickening the building operation modernization, was guaranteeing engineering construction quality, and active effect has been brought into play in protection urban and rural environment aspect.In order to guarantee the dry-mix quality product; Thereby assurance engineering construction quality; China has formulate and announced corresponding product standard to novel wall material with dry-mix, like JC860-2000 " concrete small size hollow building block masonry mortar " and JC890-2000 " steam-pressing aero-concrete is with masonry mortar and plastering mortar " etc.
On the other hand; Continuous development along with science and technology; People have proposed various new requirements to the performance of mortar, and the requirement of functions such as water-retentivity, cohesiveness, splitting resistance, water-repellancy, impermeability is being strengthened, and the invention of mortar additive solves these problems well.At present, the rate of utilization of national admixtures such as Northern Europe, Japan, Australia almost reaches 100%, and the rate of utilization that the U.S., Canada, Germany, Russia such as reach at country also is roughly 50%～80%; Other countries adopt the ratio of admixture also to grow with each passing day.
Mortar additive has kinds such as fluidizer, swelling agent, hardening accelerator, retardant, frostproofer, water-resisting agent, water reducer.Applicable cases to the existing additive for building mortar of China is studied; Find it mainly is bleed type admixture; And be representative with two types of mortar plasticizers such as rosin tree lipid and synthetic surfactants, and the actual effect of these mortar additives is unsatisfactory, exists quality problems to some extent; Mainly show as: the product that has has positive effect to the serviceability of improving mortar, but mortar strength is poor; The product that has has improved bonding strength, but bleeding is serious, denseness is poor, and serviceability is undesirable.The high-quality mortar additive plays a part very important for the performance of dry-mix; And China is applicable to that at present the special additive of dry-mix is less, and the novel high-performance mortar additive of therefore developing excellent property is that current China improves the dry-mix quality and promotes problem demanding prompt solution in the novel wall material popularization.
Being used to come from renewable resources, inexpensive, nontoxic natural high moleculer eompound develops the High Performance Mortar admixture of performances such as the diminishing enhancing that integrates good, water-proofing anticracking, bonding, insulation and will become the main developing direction of China's new wall material with dry powder mortar additive.Sulfonated lignin derive from the paper-making pulping waste liquid, are nontoxic natural high moleculer eompound, commonly used make cement water reducing agent, but water-reducing rate is low, little to ultimate compression strength raising effect.Owing to have certain diminishing and bleed effect; Sulfonated lignin also use more extensive in mortar additive, but mainly as one of constituent in the prescription, as at Chinese patent CN 1169404A; Among CN1227182C and the CN 1215013C; Air entrapment agents such as sulfonated lignin and rosin/colophonium pyrolytic polymer, sodium lauryl sulphate carry out composite, and combine hardening accelerator such as sodium sulfate, trolamine to process mortar additive, and wherein the sulfonated lignin proportion is no more than 45%.In " concrete " 2003 the 9th phases " wooden calcium sulfonate's modification prepares the experimental study of additive for compound mortar " through with composite mortar additives that is applicable to normal concrete small hollow block, autoclaved lime-sand brick and powder ash air-entrained concrete building block of preparing such as the calcium lignin sulphonate after the modification and modified rosin soap, tensio-active agent, hardening accelerator; Complex manufacturing, the sulfonated lignin utilization is few.
Summary of the invention
The objective of the invention is to overcome above-mentioned technological deficiency; With the renewable resources sulfonated lignin of originating abundant, cheap is raw material; Through attainable simple modified technique supporting high-efficiency dry powder mortar additive of a kind of and new wall material and preparation method thereof is provided; This admixture has effects such as diminishing, slow setting, bonding, bleed and water conservation; Can improve mortar strength, strengthen mortar and walling cohesiveness, improve the pore texture of mortar and strengthen its impermeability, the thermal cracking and the shrinkage crack of minimizing mortar; Its bleed effect can also reduce slurry density, helps to prepare light mortar, improves the insulation and the building energy conservation of body of wall.
The preparation method of mortar additive of the present invention is following:
(1) is the solution of concentration 30%～50% with the sulfonated lignin poach, system pH is transferred to 8.0～11.0, add urea, formaldehyde, be warming up to 80～100 ℃ of afterreactions 1～2 hour;
(2) system pH is transferred to 4.0～6.0, reacted 2～3 hours down at 80～100 ℃;
(3) add oxygenant, reacted 1～2 hour down at 70～90 ℃, cooling discharge obtains liquid product of the present invention.
Said liquid product is carried out spraying drying can obtain powder-like product.
The weight proportion of said components is following:
100 parts of sulfonated lignin
5～15 parts in urea
10～20 parts in formaldehyde
5～10 parts in oxygenant
Said sulfonated lignin are one or more in calcium lignin sulphonate, sodium lignosulfonate, the magnesium lignosulfonate.
Said oxygenant is a kind of in potassium permanganate, calcium perchlorate, the SRM 935a.
Through above-mentioned reaction; Hydroxyl, carboxyl-content in the lignosulfonic acid molecules of salt are increased; And introduce amino, its hydrophilic group content is improved, thereby after making that sulfonated lignin are adsorbed on cement particle surface; Can improve the negative charge of cement particle surface, the Coulomb repulsion effect strengthens and the raising degree of scatter; The side chain number and the molecular weight of sulfonated lignin are increased, can increase its adsorbent layer thickness at cement particle surface.Two aspect effects comprehensively improve the diminishing ability of sulfonated lignin and to the raising effect of mortar mechanical strength.Concrete reaction formula is following:
(1)
The present invention compared with prior art has the following advantages and effect:
(1) the sulfonated lignin raw material of the present invention's use is reclaimed by acid polishing effluent, and is nontoxic renewable.The production process of modification is carried out under atmospheric low-temperature, and easy handling control has the advantage that technology is simple, efficient is high, production cost is low, the ratio of performance to price is good.The spray dried prod outward appearance is a brown ceramic powder, and good water solubility belongs to green chemical.
(2) pass through modified-reaction, increase hydroxyl, carboxyl-content in the molecule, and introduce amino, its hydrophilic group content is improved, the dispersive ability enhancing of cement granules; The side chain number and the molecular weight of sulfonated lignin are increased, can increase its adsorbent layer thickness at cement particle surface.Two aspect comprehensive actions have improved the diminishing ability of sulfonated lignin and the mechanical strength of mortar.
(3) surfactivity of sulfonated lignin strengthens significantly after the modification, bubble and steady bubble ability raising, and the foam uniform and smooth; Help improving the water retention capacity of product; Overcome segregation of mortar and demixing phenomenon, reduced the shrinkability of mortar, its cracking trend is reduced; And can in mortar, introduce a large amount of pores that seal, and improve the microtexture of mortar, improve its impervious ability.
(4) after the modification in the lignosulfonic acid molecules of salt increase of carboxyl and amino content its slow setting property is strengthened to some extent, delay the hydrated cementitious thermopositive reaction, further reduce the shrinking percentage and the cracking behavior of mortar; The increase of molecular weight strengthens the cohesiveness of product, helps strengthening the cohesive strength of mortar and walling.
Description of drawings
Fig. 1 is the surface tension comparison diagram of the product of the present invention and the calcium lignin sulphonate aqueous solution;
Fig. 2 is the contrast to hydrated cementitious temperature effect of product of the present invention and calcium lignin sulphonate.
Embodiment
Embodiment 1:
Get magnesium lignosulfonate 1000g, adding water, to be made into concentration be 40% solution, adds NaOH solution system pH is transferred to 8.0, adds 100g urea, 150g formaldehyde, is heated to certain service temperature while stirring, and service temperature is controlled at 95 ℃, reacts 1 hour; Add H
2SO
4Solution transfers to 6.0 with system pH, and the conditioned reaction temperature was 90 ℃ of reactions 2 hours; Add 50g potassium permanganate, reacted 2 hours down, can obtain the liquid product of mortar additive of the present invention after the cooling, carry out spraying drying and can obtain powder-like product of the present invention at 90 ℃.
Embodiment 2:
Get sodium lignosulfonate 1000g, adding water, to be made into concentration be 50% solution, adds NaOH solution system pH is transferred to 11.0, adds 50g urea, 100g formaldehyde, is heated to certain service temperature while stirring, and service temperature is controlled at 85 ℃, reacts 1 hour; Add H
2SO
4Solution transfers to 5.0 with system pH, and the conditioned reaction temperature was 80 ℃ of reactions 3 hours; Add the 80g calcium perchlorate, the conditioned reaction temperature was reacted 1 hour down at 70 ℃, can obtain the liquid product of mortar additive of the present invention after the cooling, carried out spraying drying and can obtain powder-like product of the present invention.
Embodiment 3:
Get calcium lignin sulphonate 1000g, add water and be made into the solution into concentration 30%, add NaOH solution system pH is transferred to 9.0, add 150g urea, 200g formaldehyde, be heated to certain service temperature while stirring, service temperature is controlled at 80 ℃, reacts 2 hours; Add H
2SO
4Solution transfers to 4.0 with system pH, and the conditioned reaction temperature was reacted 2 hours down for 100 ℃ in temperature; Add the 100g SRM 935a, be warming up to 85 ℃ and reacted 1.5 hours down, can obtain the liquid product of mortar additive of the present invention after the cooling, carry out spraying drying and can obtain powder-like product of the present invention.
Embodiment 4:
Get magnesium lignosulfonate 500g, sodium lignosulfonate 500g, poach is the solution of concentration 40%, adds NaOH solution system pH is transferred to 10.0, adds 100g urea, 200g formaldehyde, is warming up to 90 ℃ of afterreactions 2 hours; Add H
2SO
4Solution transfers to 5.0 with system pH, and the conditioned reaction temperature was reacted 3 hours down for 95 ℃ in temperature; Add the 50g calcium perchlorate, reacted 0.5 hour down, can obtain the liquid product of mortar additive of the present invention after the cooling, carry out spraying drying and can obtain powder-like product of the present invention at 90 ℃.
Embodiment 5:
Getting magnesium lignosulfonate 200g, sodium lignosulfonate 400g, calcium lignin sulphonate 400g poach is the solution of concentration 40%, adds NaOH solution system pH is transferred to 9.0, adds 100g urea, 100g formaldehyde, is warming up to 90 ℃ of afterreactions 1.5 hours; Add H
2SO
4Solution transfers to 4.0 with system pH, and the conditioned reaction temperature was reacted 3 hours down for 80 ℃ in temperature; Add the 50g calcium perchlorate, reacted 2 hours down, can obtain the liquid product of mortar additive of the present invention after the cooling, carry out spraying drying and can obtain powder-like product of the present invention at 90 ℃.
Its effect has been explained in a series of tests of below using the embodiment of the invention 1 product to carry out.
1, surfactivity and latherability
Can know that from Fig. 1 the surfactivity of product of the present invention improves a lot than calcium lignin sulphonate after modification, surface tension can be reduced to 37.1mN/m when concentration was 100g/L; Corresponding with it, the latherability of product of the present invention also is improved largely than calcium lignin sulphonate, and froth stability is good, it is shattered to pieces to be difficult for.
The lathering property of table 1 mortar additive
2, mortar performance test
The hydration reaction of cement is a thermopositive reaction, and the mortar internal temperature constantly raises in this process, and when the mortar internal-external temperature difference was excessive, mortar will produce shrinkage, causes the crack to generate.Can know that from Fig. 2 during the admixture admixture, blank mortar 56 ℃ of temperature rise peak values do not occur in aquation after 12 hours, and aquation temperature peak is postponed and being occurred behind admixture calcium lignin sulphonate and the product of the present invention, and its peak value reduces.By contrast, the effect of product of the present invention is more obvious, makes warm peak reduce by 13 ℃, and postpones appearances in 37 hours, so help reducing the fissured generation of contracting of mortar temperature.
Table 2～table 4 has been listed the new sand cutting slurry of admixture product of the present invention and the performance of sclerosis mortar.Can know that from table 2 product of the present invention has higher water-reducing rate, its stronger bleed property makes the density of new sand cutting slurry increase and obviously reduce with its volume, but the bleeding of while mortar reduces, water-retentivity significantly strengthens, and helps to reduce the segregation and the layering of mortar.
The new sand cutting slurry of table 2 water-reducing rate, density ratio and bleeding rate ratio
Annotate: cement-sand ratio is 1: 3, denseness 7～8cm, and wherein density ratio, bleeding rate are 100 than all with blank sand-cement slurry
Can know from table 3 and table 4; Compare with certain mortar additive on calcium lignin sulphonate and the market " mortar is precious "; Product of the present invention can obviously improve the resistance to compression of sclerosis mortar, anti-folding and cohesive strength, and the contraction of mortar diminishes, visible crack reduces, and anti-permeability performance is improved largely.
The strength property of table 3 sclerosis mortar
Annotate: cement-sand ratio is 1: 3, the standard consistency mold filling.Because the precious bleed property of mortar is too strong; Recommend volume 0.05%～0.10% experiment generally speaking by producing house, product of the present invention has good waterproofing and anti-leakage performance, and this is determined by several respects factor: high water-reducing rate can improve the degree of compactness of mortar; Reduce drying shrinkage, improve the mechanical strength of mortar; Delayed coagulation can delay the hydrated cementitious rate of heat release, reduces or avoids temperature to contract and the generation of thermal cracking; And the bleed effect can increase mortar overall porosity, improve pore size distribution, improve petrifying water mudstone degree of compactness, to the intensity of mortar, contraction, the impervious material impact that produces.
Shrinkage value, cracking behavior and the impermeability of table 4 sclerosis mortar
Annotate: cement-sand ratio is 1: 3, the standard consistency mold filling
Claims (2)
1. preparation method who is applicable to the environment-friendly dry powder mortar additive of novel wall material is characterized in that may further comprise the steps:
(1) is the solution of concentration 30%～50% with the sulfonated lignin poach, system pH is transferred to 8.0～11.0, add urea, formaldehyde, be warming up to 80～100 ℃ of afterreactions 1～2 hour;
(2) system pH is transferred to 4.0～6.0, reacted 2～3 hours down at 80～100 ℃;
(3) add oxygenant, reacted 1～2 hour down, obtain liquid product or spraying drying after the cooling and obtain powder-like product at 70～90 ℃;
Above-mentioned raw materials weight part consumption is following:
Said sulfonated lignin are one or more in calcium lignin sulphonate, sodium lignosulfonate, the magnesium lignosulfonate;
Said oxygenant is a kind of in potassium permanganate, calcium perchlorate, the SRM 935a.
2. the mortar additive of the said method of claim 1 preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100299696A CN101391876B (en) | 2008-08-04 | 2008-08-04 | Dry powder mortar additive suitable for novel wall material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100299696A CN101391876B (en) | 2008-08-04 | 2008-08-04 | Dry powder mortar additive suitable for novel wall material and preparation method thereof |
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| Publication Number | Publication Date |
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| CN101391876A CN101391876A (en) | 2009-03-25 |
| CN101391876B true CN101391876B (en) | 2012-05-30 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180615B (en) * | 2011-03-18 | 2012-08-22 | 华南理工大学 | Modified alkali lignin cement grinding aid and preparation method thereof |
| CN102924004A (en) * | 2012-11-15 | 2013-02-13 | 上海台界化工有限公司 | Production method of dry-mixed mortar |
| CN103755211A (en) * | 2013-12-16 | 2014-04-30 | 华南理工大学 | Papermaking black liquid modification admixture for impervious mortar and preparation method thereof |
| CN105236816B (en) * | 2015-08-31 | 2017-09-26 | 华南理工大学 | It is a kind of for lignin-base additive of adhesive mortar and preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1208027A (en) * | 1998-07-21 | 1999-02-17 | 华南理工大学 | Efficient concrete water reducing agent of modified lignosulphonate and its preparation |
| CN1587176A (en) * | 2004-08-27 | 2005-03-02 | 华南理工大学 | High efficiency mortar additive for lignin series air-entraining concrete and its preparing method |
| CN1974467A (en) * | 2006-12-07 | 2007-06-06 | 华南理工大学 | Lignosulfonate series air entraining and water reducing admixture for concrete and its prepn process and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1208027A (en) * | 1998-07-21 | 1999-02-17 | 华南理工大学 | Efficient concrete water reducing agent of modified lignosulphonate and its preparation |
| CN1587176A (en) * | 2004-08-27 | 2005-03-02 | 华南理工大学 | High efficiency mortar additive for lignin series air-entraining concrete and its preparing method |
| CN1974467A (en) * | 2006-12-07 | 2007-06-06 | 华南理工大学 | Lignosulfonate series air entraining and water reducing admixture for concrete and its prepn process and application |
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