CN102863170B - Functional crystallization master batch and preparation method thereof and waterproof material - Google Patents
Functional crystallization master batch and preparation method thereof and waterproof material Download PDFInfo
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- CN102863170B CN102863170B CN 201210389184 CN201210389184A CN102863170B CN 102863170 B CN102863170 B CN 102863170B CN 201210389184 CN201210389184 CN 201210389184 CN 201210389184 A CN201210389184 A CN 201210389184A CN 102863170 B CN102863170 B CN 102863170B
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- calcium carbonate
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Abstract
The invention provides a functional crystallization master batch, a preparation method thereof and a waterproof material and belongs to the field of inorganic materials. The functional crystallization master batch is composed of a nanoscale calcium carbonate aluminum oxide composite powder body and chelated titanate. The preparation method includes preparing and mixing calcium carbonate powders and the nanoscale calcium carbonate aluminum oxide composite powder body. The waterproof material is composed of, by weight, 6-8% of the functional crystallization master batch, 4-6% of methyl cellulose thickening agents, 2-4% of anhydrous citric acids retarders, 25-35% of finely grinding quartz sands, and the balance cements. The functional crystallization master batch has excellent crystallization performance and usage performance, the preparation method is simple, low in production cost, safe in operation and suitable for industrial production, and the waterproof material has excellent impermeability pressure, compression strength and rupture strength.
Description
Technical field
The invention belongs to field of inorganic materials, relate to a kind of functional crystallization masterbatch, its preparation method and water-proof material, function of dominant inorganic materials.
Background technology
At present in field of inorganic materials, performance and the preparation of functional crystallization masterbatch has been subjected to attention.The patent No. is the patent of invention that 200410058199.X, name are called cementitious capillary waterproofing material and production technique and constructional method, a kind of cementitious capillary waterproofing material is disclosed, cement (inorganic materials) content is the 50-65% of gross weight, and all the other components are active material 5.5-14.5%, methylcellulose thickener 3.5-8.0%, Citric Acid, usp, Anhydrous Powder retardant 2.0-4.5%, levigate quartz sand 20-40%.But problem is that the effect of active material is undesirable, i.e. the performance index of material: impervious pressure, ultimate compression strength and folding strength are generally lower.
Summary of the invention
Purpose of the present invention is exactly at above-mentioned technological deficiency, and a kind of functional crystallization masterbatch is provided, and this functional crystallization masterbatch has good crystal property, and use properties is good.
Another object of the present invention provides the preparation method of above-mentioned functions crystallization masterbatch, and this preparation method's technology is simple, and production cost is low, and operational safety is suitable for suitability for industrialized production.
The objective of the invention is to be achieved through the following technical solutions:
A kind of functional crystallization masterbatch is made up of nanometer grade calcium carbonate aluminum oxide composite granule and the type titanic acid ester that boils together, and wherein the weight percentage of nanometer grade calcium carbonate aluminum oxide composite granule is 50-60%, and the weight percentage of the type that boils together titanic acid ester is 40-50%.
A kind of method for preparing described functional crystallization masterbatch comprises the steps:
(1) preparation calcium carbonate powders;
(2) preparation nanometer grade calcium carbonate aluminum oxide composite granule:
Obtained aqueous solution A: described water solution A is Al (NO
3)
3The aqueous solution;
Obtained aqueous solution B: contain NH among the described aqueous solution B
4HCO
3And polyoxyethylene glycol, NH among the described aqueous solution B
4HCO
3With the ratio of the volumetric molar concentration of polyoxyethylene glycol be 10-15:1, NH in the described solution B
4HCO
3Volumetric molar concentration and described water solution A in Al (NO
3)
3Volumetric molar concentration is identical;
Obtained aqueous solution C: described water solution A and aqueous solution B equal-volume are mixed formation aqueous solution C;
Described calcium carbonate powders is mixed with aqueous solution C, cross the leaching precipitation, behind described precipitation water successively, absolute ethanol washing, be heated to 750-850 ℃ and insulation, obtain nanometer grade calcium carbonate aluminum oxide composite granule;
(3) water is mixed with the type titanic acid ester of boiling together, 70-80 ℃ is incubated 20-30 minute, adds described nanometer grade calcium carbonate aluminum oxide composite granule then, is warming up to 110-120 ℃ and insulation, stirs 20-30 minute; After being cooled to 50-60 ℃ then, stirred 20-40 minute; Be cooled to room temperature and namely get described functional crystallization masterbatch.
The mass ratio that calcium carbonate powders and solution C described in the step (2) are mixed is 1:1-3.
Soaking time is 1.5-3 hour described in the step (2).
The weight ratio that water, the type that boils together titanic acid ester are mixed in the step (3) is 5:1-3.
The add-on of nanometer grade calcium carbonate aluminum oxide composite granule described in the step (3) be boil together type titanic acid ester weight 1-1.5 doubly.
The method for preparing calcium carbonate powders in the step (1) is: be feedstock production milk of lime with unslaked lime and water; Milk of lime and carbon dioxide reaction are obtained calcium carbonate; Described calcium carbonate powders will namely be got after the calcium carbonate drying.
The present invention also provides. a kind of water-proof material that contains described functional crystallization masterbatch, its each composition and weight percentage are: functional crystallization masterbatch 6-8%, methylcellulose thickener 4-6%, Citric Acid, usp, Anhydrous Powder retardant 2-4%, levigate quartz sand 25-35%, all the other are cement.
The present invention's beneficial effect compared to existing technology is as follows:
Nano aluminium oxide and silicate effect among the present invention generate chemical crystal, make the material densification, with formation crystal thing behind the high reactivity silicon oxide compound, can improve its self-healing performance and anti-pressure permeation function again greatly.
Nanometer grade calcium carbonate is in the material hole, forms the waterproof xln, has the effect in hydrophobic, waterproof, obstruction duct.Be that anti-the stretching of bonding drawn distortion, cracking resistance, self-healing hole hole seam, and form cracking resistance, plug-hole, waterproof layer after other material polymerization.
This material has that starting material are extensive, cost is low, nontoxic, tasteless, production formula technology is simple, waterproof construction is easy, the duration limit is short, have superpower impermeabilisation ability is difficult for destroyed; Have unique self-repairing capability free from worldly cares, can repair the crack; There is not problem of aging in the strong hydraulic pressure of energy withstand long term exposure.
The preparation method of functional crystallization masterbatch provided by the invention, technology is simple, and production cost is low, and operational safety is suitable for suitability for industrialized production.
Water-proof material provided by the invention has good impervious pressure, ultimate compression strength, folding strength.
Description of drawings
Organization chart after the functional crystallization masterbatch that Fig. 1 makes for the embodiment of the invention one is used.Can be seen the situation of forming of material by Fig. 1.
Embodiment
Below each embodiment only as explanation of the present invention.
The functional crystallization masterbatch of embodiment 1 preparation
Method one
Preparing quick lime is put in the beaker, adds water digestion.The room temperature ageing formed milk of lime in 12 hours after constant temperature stirred 0.5h then.Then pour in the carbonization reactor the milk of lime for preparing is disposable, temperature of reactor is 80 degree, and feeding gas concentration lwevel from reactor bottom is the gas of 20% (V%), and the rotating speed with 600r/ min stirs simultaneously.Stir and pour out material after 1 hour, the drying oven of putting into 105 degree then keeps taking out in 2 hours, namely obtains calcium carbonate powders.
Contain Al (NO with the deionized water preparation
3)
3Water solution A, Al (NO wherein
3)
3Concentration be 60mol/L.
With deionized water obtained aqueous solution B, wherein the concentration of NH4HCO3 is 60mol/L, and the concentration of polyoxyethylene glycol is 5mol/L.In the process for preparation, earlier that NH4HCO3 is water-soluble, add polyoxyethylene glycol again.
Solution A and solution B are mixed the formation solution C with volume.
Being 1:2 according to Paris white and solution C mass ratio mixes these two kinds of materials 1 hour, and ageing is 12 hours then.Cross the leaching precipitation, use deionized water wash 3 times, use absolute ethanol washing then 3 times, insulation obtained nanometer grade calcium carbonate aluminum oxide composite granule after 2 hours in the process furnace of 800 degree.
Water, hydramine chelating titanate (YB-405) were mixed, stir by weight 5: 2.With being heated to 70 ℃ in the solution input reactor after stirring, be incubated 20 minutes; The nanometer grade calcium carbonate aluminum oxide composite granule identical with hydramine chelating titanate (YB-405) weight joined in the reactor, be heated to 110 ℃, under the condition of insulation, stirred 30 minutes; Be cooled to 50 ℃, stirred 30 minutes, naturally cool to room temperature and can form this functional crystallization masterbatch.
Method two
Preparing quick lime is put in the beaker, adds water digestion.The room temperature ageing formed milk of lime in 12 hours after constant temperature stirred 0.5h then.Then pour in the carbonization reactor the milk of lime for preparing is disposable, temperature of reactor is 80 degree, and feeding gas concentration lwevel from reactor bottom is the gas of 20% (V%), and the rotating speed with 600r/ min stirs simultaneously.Stir and pour out material after 1 hour, the drying oven of putting into 105 degree then keeps taking out in 2 hours, namely obtains calcium carbonate powders.
Contain Al (NO with the deionized water preparation
3)
3Water solution A, Al (NO wherein
3)
3Concentration be 50mol/L.
With deionized water obtained aqueous solution B, wherein the concentration of NH4HCO3 is 50mol/L, and the concentration of polyoxyethylene glycol is 5mol/L.In the process for preparation, earlier that NH4HCO3 is water-soluble, add polyoxyethylene glycol again.
Solution A and solution B are mixed the formation solution C with volume.
Being 1:3 according to Paris white and solution C mass ratio mixes these two kinds of materials 1 hour, and ageing is 12 hours then.Cross the leaching precipitation, use deionized water wash 3 times, use absolute ethanol washing then 3 times, insulation obtained nanometer grade calcium carbonate aluminum oxide composite granule after 1.5 hours in the process furnace of 750 degree.
Water, hydramine chelating titanate (YB-405) were mixed, stir by weight 5: 3.With being heated to 75 ℃ in the solution input reactor after stirring, be incubated 25 minutes; The nanometer grade calcium carbonate aluminum oxide composite granule of 1.2 times of hydramine chelating titanate (YB-405) weight is joined in the reactor, be heated to 115 ℃, under the condition of insulation, stirred 25 minutes; Be cooled to 56 ℃, stirred 20 minutes, naturally cool to room temperature and can form this functional crystallization masterbatch.
Method three
Preparing quick lime is put in the beaker, adds water digestion.The room temperature ageing formed milk of lime in 12 hours after constant temperature stirred 0.5h then.Then pour in the carbonization reactor the milk of lime for preparing is disposable, temperature of reactor is 80 degree, and feeding gas concentration lwevel from reactor bottom is the gas of 20% (V%), and the rotating speed with 600r/ min stirs simultaneously.Stir and pour out material after 1 hour, the drying oven of putting into 105 degree then keeps taking out in 2 hours, namely obtains calcium carbonate powders.
Contain Al (NO with the deionized water preparation
3)
3Water solution A, Al (NO wherein
3)
3Concentration be 70mol/L.
With deionized water obtained aqueous solution B, wherein the concentration of NH4HCO3 is 70mol/L, and the concentration of polyoxyethylene glycol is 5mol/L.In the process for preparation, earlier that NH4HCO3 is water-soluble, add polyoxyethylene glycol again.
Solution A and solution B are mixed the formation solution C with volume.
Being 1:1 according to Paris white and solution C mass ratio mixes these two kinds of materials 1 hour, and ageing is 12 hours then.Cross the leaching precipitation, use deionized water wash 3 times, respectively wash 3 times with dehydrated alcohol then, insulation obtained nanometer grade calcium carbonate aluminum oxide composite granule after 3 hours in the process furnace of 850 degree.
Water, hydramine chelating titanate (YB-405) were mixed, stir by weight 5: 1.With being heated to 80 ℃ in the solution input reactor after stirring, be incubated 30 minutes; The nanometer grade calcium carbonate aluminum oxide composite granule of 1.5 times of hydramine chelating titanate (YB-405) weight is joined in the reactor, be heated to 120 ℃, under the condition of insulation, stirred 20 minutes; Be cooled to 60 ℃ and stirred 25 minutes, naturally cool to room temperature and can form this functional crystallization masterbatch.
Embodiment 2 preparations contain the water-proof material of functional crystallization masterbatch
Adopt the functional crystallization masterbatch of the present invention to be prepared as follows the water-proof material of prescription:
Prescription 1: functional crystallization masterbatch 6%, methylcellulose thickener 5%, Citric Acid, usp, Anhydrous Powder retardant 3%, levigate quartz sand 30%, all the other are cement.Wherein said functional crystallization masterbatch is by one preparation of embodiment 1 method.
Prescription 2: functional crystallization masterbatch 8%, methylcellulose thickener 5%, Citric Acid, usp, Anhydrous Powder retardant 3%, levigate quartz sand 30%, all the other are cement.Wherein said functional crystallization masterbatch is by two preparations of embodiment 2 methods.
Prescription 3: functional crystallization masterbatch 7%, methylcellulose thickener 5%, Citric Acid, usp, Anhydrous Powder retardant 3%, levigate quartz sand 30%, all the other are cement.Wherein said functional crystallization masterbatch is by three preparations of embodiment 3 methods.
Prescription 4: functional crystallization masterbatch 5%, methylcellulose thickener 5%, Citric Acid, usp, Anhydrous Powder retardant 3%, levigate quartz sand 30%, all the other are cement.Wherein said functional crystallization masterbatch is by one preparation of embodiment 1 method.
Prescription 5: functional crystallization masterbatch 9%, methylcellulose thickener 5%, Citric Acid, usp, Anhydrous Powder retardant 3%, levigate quartz sand 30%, all the other are cement.Wherein said functional crystallization masterbatch is by two preparations of embodiment 1 method.
Preparation method of water proof material is:
(1) cement sieves with the 0.25mm square hole sieve;
(2) quartz sand sieves with the 0.2mm square hole sieve;
(3) according to weight ratio with cement, methylcellulose gum, functional crystallization masterbatch, Citric Acid, usp, Anhydrous Powder, fine quartz sand, order is packed into and is stirred 30min in the mixer;
(4) discharging.
Detect the prepared water-proof material performance of prescription 1-5: impervious pressure (28d), ultimate compression strength (28d), folding strength (28d).Detected result such as table 1.By table 1 as seen, the performance of water-proof material within the scope of the present invention is better than the disclosed water-proof material performance of application number 200410058199.X.
But form the water-proof material that unit exceeds ratio range of the present invention, its use properties can seriously reduce.Reason is that the effect of nanometer grade calcium carbonate aluminum oxide composite granule is to generate chemical crystal, has reduced its self-healing performance and anti-pressure permeation function again, and perhaps the factor amount is too much, forms too much chemical crystal, influences the mechanical property of material.
| Sample | Composition | Impervious pressure (28d)/MPa | Ultimate compression strength (28d)/MPa | Folding strength (28d)/MPa |
| The patent No. is the material of the patent of invention preparation of 200410058199.X | Cement 50-65%, active material 2-14.5%, methylcellulose gum 3.5-8.0%, Citric Acid, usp, Anhydrous Powder 2.0-4.5%, levigate quartz sand 20-40% | 1.4 | 26.00 | ?6.80 |
| Water-proof material according to prescription 1 preparation | Prescription 1 | 1.6 | 28 | 7 |
| Water-proof material according to prescription 2 preparations | Prescription 2 | 1.7 | 30 | 7.5 |
| Water-proof material according to prescription 3 preparations | Prescription 3 | 1.6 | 30 | 7.3 |
| Water-proof material according to prescription 4 preparations | Prescription 4 | 1.3 | 25 | 6.0 |
| Water-proof material according to prescription 5 preparations | Prescription 5 | 1.5 | 28 | 5.5 |
Claims (8)
1. functional crystallization masterbatch, it is characterized in that being formed by nanometer grade calcium carbonate aluminum oxide composite granule and the type titanic acid ester that boils together, wherein the weight percentage of nanometer grade calcium carbonate aluminum oxide composite granule is 50-60%, and the weight percentage of the type that boils together titanic acid ester is 40-50%.
2. a method for preparing the described functional crystallization masterbatch of claim 1 comprises the steps:
(1) preparation calcium carbonate powders;
(2) preparation nanometer grade calcium carbonate aluminum oxide composite granule:
Obtained aqueous solution A: described water solution A is Al (NO
3)
3The aqueous solution;
Obtained aqueous solution B: contain NH among the described aqueous solution B
4HCO
3And polyoxyethylene glycol, NH among the described aqueous solution B
4HCO
3With the ratio of the volumetric molar concentration of polyoxyethylene glycol be 10-15:1, NH among the described aqueous solution B
4HCO
3Volumetric molar concentration and described water solution A in Al (NO
3)
3Volumetric molar concentration is identical;
Obtained aqueous solution C: described water solution A and aqueous solution B equal-volume are mixed formation aqueous solution C;
Described calcium carbonate powders is mixed with aqueous solution C, cross the leaching precipitation, behind described precipitation water successively, absolute ethanol washing, be heated to 750-850 ℃ and insulation, obtain nanometer grade calcium carbonate aluminum oxide composite granule;
(3) water is mixed with the type titanic acid ester of boiling together, 70-80 ℃ is incubated 20-30 minute, adds described nanometer grade calcium carbonate aluminum oxide composite granule then, stirs 20-30 minute under 110-120 ℃ of condition; After being cooled to 50-60 ℃ then, stirred 20-40 minute; Be cooled to room temperature and namely get described functional crystallization masterbatch.
3. method according to claim 2 is characterized in that: the mass ratio that calcium carbonate powders and solution C described in the step (2) are mixed is 1:1-3.
4. method according to claim 3, it is characterized in that: soaking time is 1.5-3 hour described in the step (2).
5. method according to claim 4 is characterized in that: the weight ratio that water, the type that boils together titanic acid ester are mixed in the step (3) is 5:1-3.
6. method according to claim 5 is characterized in that: the add-on of nanometer grade calcium carbonate aluminum oxide composite granule described in the step (3) be boil together type titanic acid ester weight 1-1.5 doubly.
7. method according to claim 6 is characterized in that: the method for preparing calcium carbonate powders in the step (1) is: be feedstock production milk of lime with unslaked lime and water; Milk of lime and carbon dioxide reaction are obtained calcium carbonate; Described calcium carbonate powders will namely be got after the calcium carbonate drying.
8. water-proof material that contains the described functional crystallization masterbatch of claim 1, its each composition and weight percentage are: functional crystallization masterbatch 6-8%, methylcellulose gum 4-6%, Citric Acid, usp, Anhydrous Powder 2-4%, levigate quartz sand 25-35%, all the other are cement.
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| CN106746850A (en) * | 2016-12-20 | 2017-05-31 | 安徽建筑大学 | A kind of cement base Thief zone crystallization master batch concrete and preparation method thereof |
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| CN1261385C (en) * | 2004-08-20 | 2006-06-28 | 姜哲 | Cement base permetration crystal type water-proof material and its producing process and construction method |
| WO2009146572A1 (en) * | 2008-06-02 | 2009-12-10 | 天津新技术产业园区中核防水材料有限公司 | A penetration-crystallization type cement-based water-proof material with molecular sieve structure and a method of producing the same |
| CN102718455B (en) * | 2012-07-02 | 2013-07-24 | 安徽朗凯奇建材有限公司 | Cement based capillary crystalline high-performance waterproofing powder and application thereof |
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