CN103819115B - A kind of preparation method of magnesium phosphate cement water reducer - Google Patents

A kind of preparation method of magnesium phosphate cement water reducer Download PDF

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Publication number
CN103819115B
CN103819115B CN201410007542.1A CN201410007542A CN103819115B CN 103819115 B CN103819115 B CN 103819115B CN 201410007542 A CN201410007542 A CN 201410007542A CN 103819115 B CN103819115 B CN 103819115B
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preparation
magnesium phosphate
water reducer
phosphate cement
organic solvent
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CN103819115A (en
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刘加平
缪昌文
林玮
刘建忠
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Sobute New Materials Co Ltd
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Abstract

The present invention relates to a kind of preparation method of water reducer, especially a kind of preparation method of magnesium phosphate cement water reducer.A preparation method for magnesium phosphate cement water reducer, it comprises following preparation process successively: a) organic solvent preparation: described organic solvent is made up of the raw material of following volume fraction: hexanaphthene 20-30%; Virahol 10-20%; Primary isoamyl alcohol 5-10%; Make above-mentioned raw materials blended in the water-bath of 60-70 DEG C, obtain organic solvent; B) water reducer preparation: 50-60 part organic solvent a) obtained for step and 10-15 part nonionic surface active agent are added dropwise to 5-10 part distilled water under ultrasonic vibration, obtained water reducer of the present invention.The present invention passes through the liquid form mixt of nonionic surface active agent as water reducer, improves magnesium phosphate cement mortar or concrete flowing property.

Description

A kind of preparation method of magnesium phosphate cement water reducer
Technical field
The present invention relates to a kind of preparation method of water reducer, especially a kind of preparation method of magnesium phosphate cement water reducer.
Background technology
Magnesium phosphate cement is a kind of fast hard high early strong gelling material, it is setting and harden based on the reaction between magnesium oxide and phosphate solution, there is quick setting and rapid hardening, high early strength, high-adhesive-strength, dry-shrinkage deformed little, high resistance to premium properties of waiting so long, receive and pay close attention to widely, at refractory materials, environment protection, Electronic Packaging, and all conduct a research in the field such as high temperature adhesives and apply, particularly at motorway, the Rapid-Repair of airfield runway and municipal major trunk roads, and the repairing rush construction of military engineering and the solidification aspect of objectionable impurities have broad application prospects.
But, for satisfied construction mobility needs, preparation magnesium phosphate cement mortar or concrete required water amount often substantially exceed theoretical sclerous reaction water requirement (7%), reach 20% of cement quality, even more than 30%, cause the degree of compactness of magnesium phosphate cement sill and intensity greatly to decline.And be applicable to the water reducer of silicate cement system, from series such as traditional wooden calcium based on Coulomb repulsion, sulfamate, naphthalene systems with based on sterically hindered poly carboxylic acid (PCA) series, all effective water-reduction can not be shown for magnesium phosphate cement system.Because, the process of setting of magnesium phosphate cement and silicate cement hydration process, there is huge difference, distinct two reaction process, " absorption-dispersion " effect in phosphate cement system of traditional silicate cement water reducer based on anion surfactant is subject to great suppression, can not effectively play its water-reduction.
In order to improve magnesium phosphate cement mortar or concrete mix mobility, carry out limited research from the proportioning aspect of mixture both at home and abroad.The common method taked at present by adjusting the consumption of mixing water; Meanwhile, adopt flyash to replace part magnesium phosphate cement, under the prerequisite in a disguised form improving water consumption and cement proportion, the lubrication playing flyash spheroidal particle also can play the effect of certain raising mixture mobility.But aforesaid method all can produce adverse influence to the mechanical property of magnesium phosphate cement.
Utilizing water reducer to improve cement-based material mixture is more directly effectively, and can not have the positive means of negative performance effects to performance after mortar or concrete hardening.A kind of magnesium phosphate cement compound water reducer (Wang Hongtao " Journal of Building Materials " the 1st phase in 2007), by a kind of " do not affect by pH value or affect less tensio-active agent by pH value in sour environment " and slow setting component and flyash compound, demonstrate certain water-reduction.But the early strength of use to magnesium phosphate cement sill of slow setting component and flyash has the effect of reduction, be disadvantageous to the super hardening performance of performance magnesium phosphate cement, preparation method's also relative complex that polycomponent is composite.
Summary of the invention
Object of the present invention is for the defect of prior art, by the liquid form mixt of nonionic surface active agent as water reducer, under the effect of reduction is not produced to the early strength of magnesium phosphate cement sill, improve magnesium phosphate cement mortar or concrete flowing property.For achieving the above object, adopt a kind of preparation method of magnesium phosphate cement water reducer, it comprises following preparation process successively in the present invention: a) organic solvent preparation: described organic solvent is made up of the raw material of following volume fraction: hexanaphthene 20-30%; Virahol 10-20%; Primary isoamyl alcohol 5-10%; Make above-mentioned raw materials blended in the water-bath of 60-70 DEG C, obtain organic solvent; B) water reducer preparation: 50-60 part organic solvent a) obtained for step and 10-15 part nonionic surface active agent are added dropwise to 5-10 part distilled water under ultrasonic vibration, obtained water reducer of the present invention.
The present inventor finds for naphthalene system, poly carboxylic acid series anionic surfactant is the dispersion effect of the situation silicate cement water reducer of representative does not have to(for) magnesium phosphate cement mixture, and the situation of dispersion effect is not had for above-mentioned magnesium phosphate cement mixture, first major part investigator considers to adopt is that the cats product of representative (compares nonionogenic tenside with quarternary ammonium salt compound, the wetting ability of cats product is stronger, more likely give play to the dissemination of cement granules), but experimental studies have found that, quaternary ammonium salt series cats product has certain water-reducing effect for magnesium phosphate cement mortar mixture, but water-reducing effect is very unobvious, Mortar'S Flowability is promoted to 8.5cm by 6cm.Therefore, the present inventor attempts the water reducer of use nonionogenic tenside as magnesium phosphate cement.But research finds and not all nonionogenic tenside can play good dispersion effect to magnesium phosphate cement; Finally, the comprehensive a large amount of theoretical investigation of the present inventor and experiment find that SPAN series (sorbitan fatty acid ester series) is better than cats product with TWEEN series (polyoxyethylene sorbitan fatty acid ester series) to the dissemination of magnesium phosphate cement.
The present inventor finds after further research, and due to the polymerization degree and concrete molecular structure difference, and not all SPAN series can play good dissemination with TWEEN series non-ionic type tensio-active agent to magnesium phosphate cement mixture.Therefore, after contriver studies further, find SPAN-60, SPAN-80, TWEEN-60, TWEEN-80(sorbitol anhydride oleate, sorbitan monooleate Soxylat A 25-7, sorbitan monostearate Soxylat A 25-7) etc. material single or mixture is comparatively obvious to the dispersion effect of magnesium phosphate cement mixture.
In addition, the present inventor is through further studying discovery, above-mentioned 4 kinds of materials (SPAN-60, SPAN-80, TWEEN-60, TWEEN-80) are viscous liquid, not easily in water, disperse (although have in water, have less water solubility), add in magnesium phosphate cement mixture and need longer duration of mixing competence exertion effect.But the early stage setting and harden speed of magnesium phosphate cement is very fast, needs diminishing component can play dissemination faster.Therefore, the nonionic surface active agent selected (SPAN-60, SPAN-80, TWEEN-60, TWEEN-80) is mixed with the emulsion of dispersion through research and utilization organic solvent and water by the present inventor, is joined in magnesium phosphate cement can greatly reduce dispersion magnesium phosphate cement required time by emulsion.The present inventor is applicable to the organic solvent of nonionic surface active agent of the present invention in order to the place of allotment, pass through again a large amount of time studies, by the selection of organic solvent raw material and the proportioning of raw material through a large amount of optimization, propose organic solvent, ultrasonic disperse and the distilled water dropping method feasible program that emulsion configures in this.
Component needed for the whole experiment of the present invention, operating process is all simple, greatly reduces industrial production cost, is beneficial to scale operation needs.The present invention by adding coal ash, the mode improving the proportioning of the change magnesium phosphate cement mixtures such as water consumption, does not have negative impact to the mechanical property after magnesium phosphate cement mortar or concrete sclerosis.
As preferably, described organic solvent is made up of the raw material of following volume fraction: hexanaphthene 23-28%; Virahol 13-18%; Primary isoamyl alcohol 7-9%.
The invention has the beneficial effects as follows:
(1) the present invention by stablizing the nonionic surface active agent playing dissemination in magnesium phosphate cement system, effectively dispersion magnesium phosphate cement particle, realizes magnesium phosphate cement mortar or the lifting of concrete flowing property.
(2) not by adding coal ash, the mode improving the proportioning of the change magnesium phosphate cement mixtures such as water consumption, negative impact be there is no to the mechanical property after magnesium phosphate cement mortar or concrete sclerosis.
(3) consist of relatively simple single liquid, preparation is simple, is easy to suitability for industrialized production and constructing operation.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not restricted to following embodiment.
Mortar ultimate compression strength performs with reference to GB/T17671-1999 " Test method for strength of hydraulic cement mortar (ISO method) ";
Concrete crushing strength performs with reference to GB/T50081-2002 " standard for test methods of mechanical properties of ordinary concrete ";
Mortar'S Flowability performs with reference to GB/T1346-2011 " cement normal consistency water consumption, time of coagulation, the stability method of inspection ";
Concrete slump performs with reference to GB/T50080-2002 " Standard for test methods of properties of ordinary concrete mixture standard ".
Example 1: by blended in the water-bath of 60 degrees Celsius to 20 parts of hexanaphthenes, 10 parts of Virahols and 5 parts of primary isoamyl alcohol, obtain organic solvent.By above-mentioned 50 parts of organic solvents and 10 parts of sorbitan monooleate Soxylat A 25-7s blended after, under ultrasonic vibration drip 5 parts of distilled water, prepare solution.With magnesium phosphate cement: water: sand, borax=1:0.25:3:0.05(mass ratio) mortar mixture in add above-mentioned solution stirring after 5 minutes, Mortar'S Flowability is increased to 12.5cm by 6cm.The present invention is adopted to improve the magnesium phosphate cement mortar of mobility and do not adopt 1 day ultimate compression strength of the magnesium phosphate cement mortar of water reducer to be respectively 21.7MPa and 22.0MPa, within 28 days, ultimate compression strength is respectively 51.4MPa and 50.2MPa, and use of the present invention is on the early strength (1 day) of the magnesium phosphate cement mortar of same proportioning and later strength (28 days) not impact.Illustrate that water reducer prepared by the embodiment of the present invention 1 does not affect the early strength (1 day) of magnesium phosphate cement mortar and later strength (28 days) while significantly improving sand-cement slurry dispersiveness, ensure that the result of use of water reducer prepared by the present invention.
Example 2: by blended in the water-bath of 70 degrees Celsius to 30 parts of hexanaphthenes, 20 parts of Virahols and 10 parts of primary isoamyl alcohol, obtain organic solvent.By above-mentioned 60 parts of organic solvents and 5 parts of sorbitol anhydride oleates and 10 parts of sorbitan monooleate Soxylat A 25-7s blended after, under ultrasonic vibration, drip 10 parts of distilled water, prepare solution.With magnesium phosphate cement: water: sand, borax=1:0.25:3:0.05(mass ratio) mortar mixture in add above-mentioned solution stirring after 5 minutes, Mortar'S Flowability is increased to 14cm by 6cm.
Example 3: by blended in the water-bath of 60 degrees Celsius to 25 parts of hexanaphthenes, 15 parts of Virahols and 10 parts of primary isoamyl alcohol, obtain organic solvent.By above-mentioned 55 parts of organic solvents and 5 parts of sorbitan monostearate Soxylat A 25-7s, 5 parts of sorbitol anhydride oleates and 5 parts of sorbitan monooleate Soxylat A 25-7s blended after, under ultrasonic vibration drip 10 parts of distilled water, prepare solution.With magnesium phosphate cement: water: borax: sand: stone=1:0.35:0.05:1.85:3.3(mass ratio) concrete mix in add after oily solution stirs 5 minutes, concrete degree of mobilization (slump) is increased to 11cm by 2cm.The present invention is adopted to improve the magnesium phosphate cement concrete of mobility and do not adopt the magnesium phosphate cement of water reducer concrete 1 day ultimate compression strength to be respectively 15.8MPa and 15.5MPa, within 28 days, ultimate compression strength is respectively 41.4MPa and 40.3MPa, the not impact of the concrete early strength of the magnesium phosphate cement of use of the present invention on same proportioning (1 day) and later strength (28 days).
Example 4: 30 parts of hexanaphthenes, 10 parts of Virahols, 5 parts of primary isoamyl alcohol are blended in the water-bath of 70 degrees Celsius, obtains organic solvent.By above-mentioned 60 parts of organic solvents and 5 parts of sorbitol anhydride oleates and 5 parts of s blended after, under ultrasonic vibration, drip 10 parts of distilled water, prepare solution.With magnesium phosphate cement: water: sand, borax=1:0.25:3:0.05(mass ratio) mortar mixture in add above-mentioned solution stirring after 5 minutes, Mortar'S Flowability is increased to 11.5cm by 6cm.
Comparative example 1
With magnesium phosphate cement: water: sand, borax=1:0.25:3:0.05(mass ratio) mortar mixture in add after naphthalenesulfonate series water reducer stirs 5 minutes, Mortar'S Flowability is still 6cm.
Comparative example 2
With magnesium phosphate cement: water: sand, borax=1:0.25:3:0.05(mass ratio) mortar mixture in add after poly carboxylic acid series water reducer stirs 5 minutes, Mortar'S Flowability is still 6cm.
Do not promote from the Mortar'S Flowability of the control sample of comparative example 1 and the known employing naphthalenesulfonate of comparative example 2 and poly carboxylic acid series water reducer.

Claims (2)

1. a preparation method for magnesium phosphate cement water reducer, is characterized in that it comprises following preparation process successively:
A) organic solvent preparation:
Described organic solvent is made up of the raw material of following volume parts:
Hexanaphthene 20-30,
Virahol 10-20,
Primary isoamyl alcohol 5-10;
Make above-mentioned raw materials blended in the water-bath of 60-70 DEG C, obtain organic solvent;
B) water reducer preparation:
50-60 part organic solvent a) obtained for step and 10-15 part nonionic surface active agent are added dropwise to 5-10 part distilled water under ultrasonic vibration, obtained described water reducer; Described " part " refers to parts by volume;
Step b) described nonionic surface active agent is at least one in sorbitol anhydride oleate, sorbitan monooleate Soxylat A 25-7, sorbitan monostearate Soxylat A 25-7.
2. the preparation method of a kind of magnesium phosphate cement water reducer as claimed in claim 1, is characterized in that: described organic solvent is made up of the raw material of following volume parts:
Hexanaphthene 23-28,
Virahol 13-18,
Primary isoamyl alcohol 7-9.
CN201410007542.1A 2014-01-08 2014-01-08 A kind of preparation method of magnesium phosphate cement water reducer Active CN103819115B (en)

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CN109776006A (en) * 2019-03-15 2019-05-21 中电投工程研究检测评定中心有限公司 A kind of magnesium phosphate cement and concrete
CN114644741B (en) * 2020-12-21 2023-10-31 博特新材料泰州有限公司 Amphoteric phosphonate water reducer, preparation method and application thereof
CN112723783B (en) * 2021-01-29 2022-09-16 江苏奥莱特新材料股份有限公司 Organic-inorganic composite retarder suitable for magnesium phosphate repair material

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CN101146751A (en) * 2005-03-30 2008-03-19 株式会社日本触媒 Cement admixture
CN101547874A (en) * 2006-12-06 2009-09-30 建筑研究和技术有限公司 Rheology modifying additive for cementitious compositions

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JP2007191334A (en) * 2006-01-18 2007-08-02 Denki Kagaku Kogyo Kk Cement admixture, cement composition and method of producing centrifugal casting product using the same

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Address after: No.6 shuiyougang, Gulou District, Nanjing City, Jiangsu Province 210013

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Patentee before: JIANGSU SUBOTE NEW MATERIALS Co.,Ltd.