CN107903565A - A kind of high performance polycarboxylate water-reducer and preparation method thereof - Google Patents

A kind of high performance polycarboxylate water-reducer and preparation method thereof Download PDF

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CN107903565A
CN107903565A CN201711220624.4A CN201711220624A CN107903565A CN 107903565 A CN107903565 A CN 107903565A CN 201711220624 A CN201711220624 A CN 201711220624A CN 107903565 A CN107903565 A CN 107903565A
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product
parts
obtains
added dropwise
kettle
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郎剑雷
金利学
徐琴
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ZHEJIANG DADONGWU GROUP CONSTRUCTION NEW MATERIALS CO Ltd
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ZHEJIANG DADONGWU GROUP CONSTRUCTION NEW MATERIALS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16Sulfur-containing compounds
    • C04B24/18Lignin sulfonic acid or derivatives thereof, e.g. sulfite lye
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • C04B24/26Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B24/2605Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F289/00Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L51/00Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L51/08Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/327Aluminium phosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention discloses a kind of high performance polycarboxylate water-reducer and preparation method thereof, it is made of with following raw materials, acrylic acid, thioacetic acid, isoamyl alcohol polyoxyethylene ether, hydrogen peroxide, vitamin, white sugar, dodecyl sodium sulfate, solid naphthalene, the concentrated sulfuric acid, formaldehyde, liquid caustic soda, polyethylene glycol monomethyl ethermethacrylic acid esters, calcium lignosulfonate, SYNPERONIC PE/F68, trehalose, silicone powder, shale ashes, sodium hydrogensulfite, polyethylene glycol oxide, aluminium triphosphate, cocounut oil acyl diethanol amine, dinonyl naphthalene sulfonate barium, methenamine, auxiliary agent, acetone, sodium sulfite, acrylamide, initiator, water;Its preparation method is to mix isoamyl alcohol polyoxyethylene ether etc.;Add the stirring such as silicone powder after solid naphthalene is processed;Acrylamide etc. is processed;Finally product three times is mixed, up to a kind of high performance polycarboxylate water-reducer.The present invention can not only improve corrosion resistance and water-reducing rate, also have the advantages that slump-loss is less.

Description

A kind of high performance polycarboxylate water-reducer and preparation method thereof
Technical field
The present invention relates to water-reducing agent field, particularly a kind of high performance polycarboxylate water-reducer and preparation method thereof.
Background technology
Polycarboxylate water-reducer be in the market application prospect preferably, preferably a kind of cement water reducing agent of comprehensive performance, but its Corrosion resistance is poor, and can also have much room for improvement on water-reducing rate and the slump, further to meet the needs of market.Therefore, it is existing There is the problem of corrosion resistance is poor, water-reducing rate is relatively low and slump-loss is larger for some polycarboxylate water-reducers.
The content of the invention
It is an object of the present invention to provide a kind of high performance polycarboxylate water-reducer and preparation method thereof.The present invention is not only Corrosion resistance and water-reducing rate can be improved, also has the advantages that slump-loss is less.
Technical scheme:A kind of high performance polycarboxylate water-reducer, it is with the raw material system of following weight proportions Into,
18~26 parts of acrylic acid, 8~14 parts of thioacetic acid, 18~34 parts of isoamyl alcohol polyoxyethylene ether, hydrogen peroxide 1~ 7 parts, 1~7 part of vitamin C, 1~3 part of white sugar, 0.2~0.8 part of dodecyl sodium sulfate, 80~90 parts of solid naphthalene, the concentrated sulfuric acid 80 ~120 parts, 30~42 parts of formaldehyde, 30~40 parts of liquid caustic soda, 14~22 parts of polyethylene glycol monomethyl ethermethacrylic acid esters, sulfomethylated lignin Sour 10~20 parts of calcium, 8~12 parts of ethylene oxide-propylene oxide copolymer, 1~3 part of trehalose, 1~2 part of silicone powder, shale ashes 2.5~6.5 parts, 1.5~3.5 parts of sodium hydrogensulfite, 4~8 parts of polyethylene glycol oxide, 6.5~10.5 parts of aluminium triphosphate, cocounut oil acyl 2~4 parts of diethanol amine, 0.5~1.5 part of dinonyl naphthalene sulfonate barium, 1~3 part of methenamine, 0.5~1.5 part of auxiliary agent, acetone 35 ~55 parts, 80~180 parts of sodium sulfite, 10~30 parts of acrylamide, 2~7 parts of initiator, 300~500 parts of water.
In a kind of foregoing high performance polycarboxylate water-reducer, the auxiliary agent be made of with the raw material of following weight proportions,
10~20 parts of magnesia, 4~8 parts of Humic acid Magnesium, 3~6 parts of ammonium benzoate, 9~15 parts of α-sodium olefin sulfonate, inositol Six 2~4 parts of phosphates, 3~7 parts of isobutene triethoxysilane, 8~12 parts of poly-ferric chloride, 15~21 parts of germanite powder, titanium white 8~12 parts of powder, 1~3 part of myristyl glucoside, 6~9 parts of polyamide wax, 3~5 parts of lithium magnesium silicate, Tea Saponin 1.5~4.5 Part.
In a kind of foregoing high performance polycarboxylate water-reducer, the initiator is persulfate, including potassium peroxydisulfate, mistake Any one or more in sodium sulphate and ammonium persulfate.
A kind of preparation method of high performance polycarboxylate water-reducer as the aforementioned, comprises the following steps:
A, isoamyl alcohol polyoxyethylene ether is put into agitator tank with water and stirred evenly, obtain A product;
B, at low ambient temperatures toward sequentially adding acrylic acid, thioacetic acid, hydrogen peroxide, vitamin C, liquid caustic soda, white in A product Sugar and dodecyl sodium sulfate, are mixed, obtain B product;
C, B product are filtered and drying and processing, obtains C product;
D, thawing processing is carried out to solid naphthalene, will be heated in solid naphthalene inputization naphthalene kettle, solid naphthalene is heated to 80 DEG C Shi Ronghua, obtains D product;
E, sulfonation processing is carried out to D product, D product is positioned in sulphonation kettle with the concentrated sulfuric acid and are reacted, are reacted in sulphonation kettle Time be 3h, the temperature reacted in sulphonation kettle is 160~165 DEG C, obtains E product;
F, cooling treatment is carried out to E product, is hydrolyzed after E product are cooled down, obtains F product;
G, condensation processing is carried out to F product, F product is positioned in condensation kettle, formaldehyde is added in condensation kettle and is reacted, is obtained G product;
H, G product are neutralized, G product is positioned over and are neutralized in kettle, in and liquid caustic soda is added dropwise in kettle, obtains H product;
I, H product are filtered and drying and processing, obtains I product;
J, auxiliary agent is added into I product, stirs evenly, obtain J product;
K, toward sequentially adding polyethylene glycol monomethyl ethermethacrylic acid esters, calcium lignosulfonate, ethylene oxide-ring in J product Ethylene Oxide copolymer, trehalose, silicone powder, shale ashes, sodium hydrogensulfite, polyethylene glycol oxide, aluminium triphosphate, cocounut oil acyl diethyl Hydramine, dinonyl naphthalene sulfonate barium and methenamine, are mixed, and obtain K product;
L, K product are filtered and pressure spray dryer is handled, obtain L product;
M, acrylamide, sodium sulfite and water are positioned in reaction kettle, are warming up to 50~55 DEG C of dissolvings, then be at the uniform velocity added dropwise Formaldehyde, 1h are dripped off, then cooling discharging, obtain M product;
N, water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle, then acetone is added dropwise, add initiator, then drip Add formaldehyde, M product are then added dropwise, finally add water and cool down, obtain N product;
O, N product are filtered and drying and processing, obtains O product;
P, C product, L product and 0 product are stirred evenly, obtains finished product.
In foregoing preparation method, the auxiliary agent in the step g is prepared by following steps,
A1, mixed magnesia, germanite powder, titanium dioxide, obtains A1 product;
B1, toward sequentially adding α-sodium olefin sulfonate, isobutene triethoxysilane, polyamide wax and magnesium silicate in A1 product Lithium, is mixed, and obtains B1 product;
B1 product, is positioned over 10~14min of stirring under 40~60 DEG C of bath temperatures by c1, is cooled to room temperature, is obtained C1 product;
D1, toward sequentially adding Humic acid Magnesium, ammonium benzoate, inositol hexaphosphate, poly-ferric chloride, myristyl in C1 product Glucoside and Tea Saponin stirring, are mixed, obtain finished product.
In foregoing preparation method, low temperature environment is 5~20 DEG C in the step b;E product are carried out in the step f cold But, make E product cool to 120 DEG C to be hydrolyzed again, hydrolysis time 0.5h.
In foregoing preparation method, in the step h in and in kettle during dropwise addition liquid caustic soda, until neutralizing the pH value position in kettle When 7~9, stop that liquid caustic soda is added dropwise;Pressure spray dryer, which is handled, in the step l is, using high-pressure pump, with the pressure of 150Mpa Power, by material by atomizer, the dimerization particulate that nebulizes directly is contacted with hot-air, carries out heat exchange, and the short time completes drying.
In foregoing preparation method, in the step m when formaldehyde is added dropwise, the temperature control during dropwise addition is 68~72 DEG C, drip off follow-up continuation of insurance temperature 3h.
In foregoing preparation method, be in the step n water is positioned in another reaction kettle with sodium sulfite stir it is molten Solution, then acetone is at the uniform velocity added dropwise, 0.5h is dripped off;Initiator is added, then formaldehyde is at the uniform velocity added dropwise, 2h is dripped off, while M product are added dropwise, and is controlled Temperature processed is 90~95 DEG C, then keeps the temperature 2h;Finally plus water and it is cooled to less than 40 DEG C, obtains N product.
In foregoing preparation method, the number and step of formaldehyde is added dropwise in the step g in the number of dropwise addition formaldehyde, step m The number all same of formaldehyde is added dropwise in rapid n.
Compared with prior art, present invention improves over existing polycarboxylate water-reducer and preparation method thereof so that the present invention Corrosion resistance is good, water-reducing rate is high, and water-reducing rate is high by up to 50%, can obviously improve concrete flowability, can make the identical ratio of mud Concrete slump gradual loss it is small, 70min does not lose substantially, 100min loss 10-20%, concrete can be increased substantially The intensity of each age, suitable for all kinds of concrete;By the introducing of modified monomer acrylamide, water-reducing agent is further increased Water-reducing rate, the slump-loss for reducing concrete, and make its cement adaptability more preferable;It is obvious to concrete enhancing effect, collapse Degree of falling loss is small, and low temperature, suitable for low temperature environment, improves the scope of application without sulfate crystal phenomenon.Therefore, the present invention not only Corrosion resistance and water-reducing rate can be improved, improve mobility, also have the advantages that slump-loss is smaller and the scope of application is wider.
Embodiment
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
Embodiment one.A kind of high performance polycarboxylate water-reducer, is made with the raw material of following weight proportions,
18~26 parts of acrylic acid, 8~14 parts of thioacetic acid, 18~34 parts of isoamyl alcohol polyoxyethylene ether, hydrogen peroxide 1~ 7 parts, 1~7 part of vitamin C, 1~3 part of white sugar, 0.2~0.8 part of dodecyl sodium sulfate, 80~90 parts of solid naphthalene, the concentrated sulfuric acid 80 ~120 parts, 30~42 parts of formaldehyde, 30~40 parts of liquid caustic soda, 14~22 parts of polyethylene glycol monomethyl ethermethacrylic acid esters, sulfomethylated lignin Sour 10~20 parts of calcium, 8~12 parts of ethylene oxide-propylene oxide copolymer, 1~3 part of trehalose, 1~2 part of silicone powder, shale ashes 2.5~6.5 parts, 1.5~3.5 parts of sodium hydrogensulfite, 4~8 parts of polyethylene glycol oxide, 6.5~10.5 parts of aluminium triphosphate, cocounut oil acyl 2~4 parts of diethanol amine, 0.5~1.5 part of dinonyl naphthalene sulfonate barium, 1~3 part of methenamine, 0.5~1.5 part of auxiliary agent, acetone 35 ~55 parts, 80~180 parts of sodium sulfite, 10~30 parts of acrylamide, 2~7 parts of initiator, 300~500 parts of water.
The auxiliary agent be made of with the raw material of following weight proportions,
10~20 parts of magnesia, 4~8 parts of Humic acid Magnesium, 3~6 parts of ammonium benzoate, 9~15 parts of α-sodium olefin sulfonate, inositol Six 2~4 parts of phosphates, 3~7 parts of isobutene triethoxysilane, 8~12 parts of poly-ferric chloride, 15~21 parts of germanite powder, titanium white 8~12 parts of powder, 1~3 part of myristyl glucoside, 6~9 parts of polyamide wax, 3~5 parts of lithium magnesium silicate, Tea Saponin 1.5~4.5 Part.
The initiator be in persulfate, including potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate any one or it is more Kind.
A kind of preparation method of high performance polycarboxylate water-reducer, comprises the following steps:
A, isoamyl alcohol polyoxyethylene ether is put into agitator tank with water and stirred evenly, obtain A product;
B, at low ambient temperatures toward sequentially adding acrylic acid, thioacetic acid, hydrogen peroxide, vitamin C, liquid caustic soda, white in A product Sugar and dodecyl sodium sulfate, are mixed, obtain B product;
C, B product are filtered and drying and processing, obtains C product;
D, thawing processing is carried out to solid naphthalene, will be heated in solid naphthalene inputization naphthalene kettle, solid naphthalene is heated to 80 DEG C Shi Ronghua, obtains D product;
E, sulfonation processing is carried out to D product, D product is positioned in sulphonation kettle with the concentrated sulfuric acid and are reacted, are reacted in sulphonation kettle Time be 3h, the temperature reacted in sulphonation kettle is 160~165 DEG C, obtains E product;
F, cooling treatment is carried out to E product, is hydrolyzed after E product are cooled down, obtains F product;
G, condensation processing is carried out to F product, F product is positioned in condensation kettle, formaldehyde is added in condensation kettle and is reacted, is obtained G product;
H, G product are neutralized, G product is positioned over and are neutralized in kettle, in and liquid caustic soda is added dropwise in kettle, obtains H product;
I, H product are filtered and drying and processing, obtains I product;
J, auxiliary agent is added into I product, stirs evenly, obtain J product;
K, toward sequentially adding polyethylene glycol monomethyl ethermethacrylic acid esters, calcium lignosulfonate, ethylene oxide-ring in J product Ethylene Oxide copolymer, trehalose, silicone powder, shale ashes, sodium hydrogensulfite, polyethylene glycol oxide, aluminium triphosphate, cocounut oil acyl diethyl Hydramine, dinonyl naphthalene sulfonate barium and methenamine, are mixed, and obtain K product;
L, K product are filtered and pressure spray dryer is handled, obtain L product;
M, acrylamide, sodium sulfite and water are positioned in reaction kettle, are warming up to 50~55 DEG C of dissolvings, then be at the uniform velocity added dropwise Formaldehyde, 1h are dripped off, then cooling discharging, obtain M product;
N, water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle, then acetone is added dropwise, add initiator, then drip Add formaldehyde, M product are then added dropwise, finally add water and cool down, obtain N product;
O, N product are filtered and drying and processing, obtains O product;
P, C product, L product and 0 product are stirred evenly, obtains finished product.
Auxiliary agent in the step g is prepared by following steps,
A1, mixed magnesia, germanite powder, titanium dioxide, obtains A1 product;
B1, toward sequentially adding α-sodium olefin sulfonate, isobutene triethoxysilane, polyamide wax and magnesium silicate in A1 product Lithium, is mixed, and obtains B1 product;
B1 product, is positioned over 10~14min of stirring under 40~60 DEG C of bath temperatures by c1, is cooled to room temperature, is obtained C1 product;
D1, toward sequentially adding Humic acid Magnesium, ammonium benzoate, inositol hexaphosphate, poly-ferric chloride, myristyl in C1 product Glucoside and Tea Saponin stirring, are mixed, obtain finished product.
Low temperature environment is 5~20 DEG C in the step b;E product are cooled down in the step f, make E product cool to 120 DEG C are hydrolyzed again, hydrolysis time 0.5h;In the step h in and in kettle during dropwise addition liquid caustic soda, until neutralizing in kettle When pH value is located at 7~9, stop that liquid caustic soda is added dropwise;Pressure spray dryer, which is handled, in the step l is, using high-pressure pump, with 150Mpa Pressure, by material by atomizer, the dimerization particulate that nebulizes directly is contacted with hot-air, carries out heat exchange, and the short time completes It is dry;In the step m when formaldehyde is added dropwise, the temperature control during dropwise addition drips off follow-up continuation of insurance temperature 3h at 68~72 DEG C; It is that water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle in the step n, then acetone is at the uniform velocity added dropwise, 0.5h drops It is complete;Initiator is added, then formaldehyde is at the uniform velocity added dropwise, 2h is dripped off, while M product are added dropwise, and controlled at 90~95 DEG C, is then kept the temperature 2h;Finally plus water and it is cooled to less than 40 DEG C, obtains N product;Formaldehyde is added dropwise in the number of dropwise addition formaldehyde, step m in the step g The number all same of formaldehyde is added dropwise in number and step n.
Embodiment two.A kind of high performance polycarboxylate water-reducer, is made with the raw material of following weight proportions,
20~24 parts of acrylic acid, 10~12 parts of thioacetic acid, 24~28 parts of isoamyl alcohol polyoxyethylene ether, hydrogen peroxide 3 ~5 parts, it is 3~5 parts of vitamin C, 1.8~2.2 parts of white sugar, 0.4~0.6 part of dodecyl sodium sulfate, 83~87 parts of solid naphthalene, dense 90~110 parts of sulfuric acid, 33~39 parts of formaldehyde, 33~37 parts of liquid caustic soda, 16~20 parts of polyethylene glycol monomethyl ethermethacrylic acid esters, wood 13~17 parts of quality sulfoacid calcium, 9~11 parts of ethylene oxide-propylene oxide copolymer, 1.5~2.5 parts of trehalose, silicone powder 1.2 ~1.8 parts, 3.5~5.5 parts of shale ashes, 2~3 parts of sodium hydrogensulfite, 5~7 parts of polyethylene glycol oxide, aluminium triphosphate 7.5~9.5 Part, 2.5~3.5 parts of cocounut oil acyl diethanol amine, 0.8~1.2 part of dinonyl naphthalene sulfonate barium, 1.5~2.5 parts of methenamine, auxiliary agent 0.8~1.2 part, 40~50 parts of acetone, 110~150 parts of sodium sulfite, 15~25 parts of acrylamide, 3~6 parts of initiator, water 350~450 parts.
The auxiliary agent be made of with the raw material of following weight proportions,
13~17 parts of magnesia, 5~7 parts of Humic acid Magnesium, 4~5 parts of ammonium benzoate, 11~13 parts of α-sodium olefin sulfonate, flesh 2.5~3.5 parts of six phosphate of alcohol, 4~6 parts of isobutene triethoxysilane, 9~11 parts of poly-ferric chloride, germanite powder 17~19 Part, 9~11 parts of titanium dioxide, 1.5~2.5 parts of myristyl glucoside, 7~8 parts of polyamide wax, 3.5~4.5 parts of lithium magnesium silicate, 2.5~3.5 parts of Tea Saponin.
The initiator be in persulfate, including potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate any one or it is more Kind.
A kind of preparation method of high performance polycarboxylate water-reducer, comprises the following steps:
A, isoamyl alcohol polyoxyethylene ether is put into agitator tank with water and stirred evenly, obtain A product;
B, at low ambient temperatures toward sequentially adding acrylic acid, thioacetic acid, hydrogen peroxide, vitamin C, liquid caustic soda, white in A product Sugar and dodecyl sodium sulfate, are mixed, obtain B product;
C, B product are filtered and drying and processing, obtains C product;
D, thawing processing is carried out to solid naphthalene, will be heated in solid naphthalene inputization naphthalene kettle, solid naphthalene is heated to 80 DEG C Shi Ronghua, obtains D product;
E, sulfonation processing is carried out to D product, D product is positioned in sulphonation kettle with the concentrated sulfuric acid and are reacted, are reacted in sulphonation kettle Time be 3h, the temperature reacted in sulphonation kettle is 161~164 DEG C, obtains E product;
F, cooling treatment is carried out to E product, is hydrolyzed after E product are cooled down, obtains F product;
G, condensation processing is carried out to F product, F product is positioned in condensation kettle, formaldehyde is added in condensation kettle and is reacted, is obtained G product;
H, G product are neutralized, G product is positioned over and are neutralized in kettle, in and liquid caustic soda is added dropwise in kettle, obtains H product;
I, H product are filtered and drying and processing, obtains I product;
J, auxiliary agent is added into I product, stirs evenly, obtain J product;
K, toward sequentially adding polyethylene glycol monomethyl ethermethacrylic acid esters, calcium lignosulfonate, ethylene oxide-ring in J product Ethylene Oxide copolymer, trehalose, silicone powder, shale ashes, sodium hydrogensulfite, polyethylene glycol oxide, aluminium triphosphate, cocounut oil acyl diethyl Hydramine, dinonyl naphthalene sulfonate barium and methenamine, are mixed, and obtain K product;
L, K product are filtered and pressure spray dryer is handled, obtain L product;
M, acrylamide, sodium sulfite and water are positioned in reaction kettle, are warming up to 51~54 DEG C of dissolvings, then be at the uniform velocity added dropwise Formaldehyde, 1h are dripped off, then cooling discharging, obtain M product;
N, water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle, then acetone is added dropwise, add initiator, then drip Add formaldehyde, M product are then added dropwise, finally add water and cool down, obtain N product;
O, N product are filtered and drying and processing, obtains O product;
P, C product, L product and 0 product are stirred evenly, obtains finished product.
Auxiliary agent in the step g is prepared by following steps,
A1, mixed magnesia, germanite powder, titanium dioxide, obtains A1 product;
B1, toward sequentially adding α-sodium olefin sulfonate, isobutene triethoxysilane, polyamide wax and magnesium silicate in A1 product Lithium, is mixed, and obtains B1 product;
B1 product, is positioned over 11~13min of stirring under 45~55 DEG C of bath temperatures by c1, is cooled to room temperature, is obtained C1 product;
D1, toward sequentially adding Humic acid Magnesium, ammonium benzoate, inositol hexaphosphate, poly-ferric chloride, myristyl in C1 product Glucoside and Tea Saponin stirring, are mixed, obtain finished product.
Low temperature environment is 9~16 DEG C in the step b;E product are cooled down in the step f, make E product cool to 120 DEG C are hydrolyzed again, hydrolysis time 0.5h;In the step h in and in kettle during dropwise addition liquid caustic soda, until neutralizing in kettle When pH value is located at 7~8, stop that liquid caustic soda is added dropwise;Pressure spray dryer, which is handled, in the step l is, using high-pressure pump, with 150Mpa Pressure, by material by atomizer, the dimerization particulate that nebulizes directly is contacted with hot-air, carries out heat exchange, and the short time completes It is dry;In the step m when formaldehyde is added dropwise, the temperature control during dropwise addition drips off follow-up continuation of insurance temperature 3h at 69~71 DEG C; It is that water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle in the step n, then acetone is at the uniform velocity added dropwise, 0.5h drops It is complete;Initiator is added, then formaldehyde is at the uniform velocity added dropwise, 2h is dripped off, while M product are added dropwise, and controlled at 91~94 DEG C, is then kept the temperature 2h;Finally plus water and it is cooled to less than 40 DEG C, obtains N product;Formaldehyde is added dropwise in the number of dropwise addition formaldehyde, step m in the step g The number all same of formaldehyde is added dropwise in number and step n.
Embodiment three.A kind of high performance polycarboxylate water-reducer, is made with the raw material of following weight proportions,
22 parts of acrylic acid, 11 parts of thioacetic acid, 26 parts of isoamyl alcohol polyoxyethylene ether, 4 parts of hydrogen peroxide, vitamin C 4 Part, 2 parts of white sugar, 0.5 part of dodecyl sodium sulfate, 85 parts of solid naphthalene, 100 parts of the concentrated sulfuric acid, 36 parts of formaldehyde, 35 parts of liquid caustic soda, poly- second 18 parts of glycol monomethyl ether methacrylate, 15 parts of calcium lignosulfonate, 10 parts of ethylene oxide-propylene oxide copolymer, seaweed Sugar 2 parts, 1.5 parts of silicone powder, 4.5 parts of shale ashes, 2.5 parts of sodium hydrogensulfite, 6 parts of polyethylene glycol oxide, 8.5 parts of aluminium triphosphate, 3 parts of cocounut oil acyl diethanol amine, 1 part of dinonyl naphthalene sulfonate barium, 2 parts of methenamine, 1 part of auxiliary agent, 45 parts of acetone, sodium sulfite 130 Part, 20 parts of acrylamide, 4.5 parts of initiator, 400 parts of water.
The auxiliary agent be made of with the raw material of following weight proportions,
15 parts of magnesia, 6 parts of Humic acid Magnesium, 4.5 parts of ammonium benzoate, 12 parts of α-sodium olefin sulfonate, inositol hexaphosphate 3 Part, 5 parts of isobutene triethoxysilane, 10 parts of poly-ferric chloride, 18 parts of germanite powder, 10 parts of titanium dioxide, myristyl glucoside 2 Part, 7.5 parts of polyamide wax, 4 parts of lithium magnesium silicate, 3 parts of Tea Saponin.
The initiator be in persulfate, including potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate any one or it is more Kind.
A kind of preparation method of high performance polycarboxylate water-reducer, comprises the following steps:
A, 26 parts of isoamyl alcohol polyoxyethylene ethers are put into agitator tank with 40 parts of water and stirred evenly, obtain A product;
B, at low ambient temperatures toward sequentially add in A product 22 parts of acrylic acid, 11 parts of thioacetic acid, 4 parts of hydrogen peroxide, 4 parts Vitamin C, 5 parts of liquid caustic soda, 2 parts of white sugar and 0.5 part of dodecyl sodium sulfate, are mixed, obtain B product;
C, B product are filtered and drying and processing, obtains C product;
D, thawing processing is carried out to 85 solid naphthalenes, will be heated in 85 parts of solid naphthalene inputization naphthalene kettles, 85 parts of solid naphthalenes It is heated to melting at 80 DEG C, obtains D product;
E, sulfonation processing is carried out to D product, D product is positioned in sulphonation kettle with 100 parts of concentrated sulfuric acids and are reacted, in sulphonation kettle The time of reaction is 3h, and the temperature reacted in sulphonation kettle is 163 DEG C, obtains E product;
F, cooling treatment is carried out to E product, is hydrolyzed after E product are cooled down, obtains F product;
G, condensation processing is carried out to F product, F product is positioned in condensation kettle, 12 parts of formaldehyde are added in condensation kettle and are carried out instead Should, obtain G product;
H, G product are neutralized, G product is positioned over and are neutralized in kettle, 15 parts of liquid caustic soda are added dropwise in and in kettle, obtain H product;
I, H product are filtered and drying and processing, obtains I product;
J, 1 part of auxiliary agent is added into I product, stirs evenly, obtain J product;
K, toward sequentially add in J product 18 parts of polyethylene glycol monomethyl ethermethacrylic acid esters, 15 parts of calcium lignosulfonates, 10 parts Ethylene oxide-propylene oxide copolymer, 2 portions of trehaloses, 1.5 parts of silicone powders, 4.5 parts of shale ashes, 2.5 parts of sodium hydrogensulfites, 6 parts Polyethylene glycol oxide, 8.5 parts of aluminium triphosphates, 3 parts of cocounut oil acyl diethanol amine, 1 part of dinonyl naphthalene sulfonate barium and 2 parts of methenamines, Mixed, obtain K product;
L, K product are filtered and pressure spray dryer is handled, obtain L product;
M, 20 parts of acrylamides, 65 parts of sodium sulfites and 180 parts of water are positioned in reaction kettle, are warming up to 52 DEG C of dissolvings, 12 parts of formaldehyde are at the uniform velocity added dropwise again, 1h is dripped off, and then cooling discharging, obtains M product;
N, 180 parts of water and 65 parts of sodium sulfites are positioned over stirring and dissolving in another reaction kettle, then 45 parts of acetone is added dropwise, added Enter 4.5 parts of initiators, then 12 parts of formaldehyde are added dropwise, M product are then added dropwise, finally add water and cool down, obtain N product;
O, N product are filtered and drying and processing, obtains O product;
P, C product, L product and 0 product are stirred evenly, obtains finished product.
Auxiliary agent in the step g is prepared by following steps,
A1, mixed 15 parts of magnesias, 18 parts of germanite powder, 10 parts of titanium dioxides, obtains A1 product;
B1, toward sequentially adding 12 parts of α-sodium olefin sulfonates, 5 parts of isobutene triethoxysilanes, 7.5 parts of polyamide in A1 product Wax and 4 parts of lithium magnesium silicates, are mixed, obtain B1 product;
B1 product, be positioned under 50 DEG C of bath temperatures and stir 12min by c1, is cooled to room temperature, obtains C1 product;
D1, toward sequentially adding 6 parts of Humic acid Magnesiums, 4.5 parts of ammonium benzoates, 3 parts of inositol hexaphosphates, 10 parts of polymerizations in C1 product Iron chloride, 2 parts of myristyl glucosides and 3 parts of Tea Saponin stirrings, are mixed, obtain finished product.
Low temperature environment is 13 DEG C in the step b;E product are cooled down in the step f, E product is cooled to 120 DEG C it is hydrolyzed again, hydrolysis time 0.5h;In the step h in and in kettle during dropwise addition liquid caustic soda, until neutralizing the PH in kettle When value is located at 7, stop that liquid caustic soda is added dropwise;Pressure spray dryer, which is handled, in the step l is, using high-pressure pump, with the pressure of 150Mpa Power, by material by atomizer, the dimerization particulate that nebulizes directly is contacted with hot-air, carries out heat exchange, and the short time completes drying; In the step m when formaldehyde is added dropwise, the temperature control during dropwise addition drips off follow-up continuation of insurance temperature 3h at 70 DEG C;The step n In be that water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle, then acetone is at the uniform velocity added dropwise, 0.5h is dripped off;Addition is drawn Agent is sent out, then formaldehyde is at the uniform velocity added dropwise, 2h is dripped off, while M product are added dropwise, and controlled at 92 DEG C, then keeps the temperature 2h;Finally plus water simultaneously Less than 40 DEG C are cooled to, obtains N product;It is added dropwise in the step g in the number of dropwise addition formaldehyde, step m in the number and step n of formaldehyde The number all same of formaldehyde is added dropwise.

Claims (10)

  1. A kind of 1. high performance polycarboxylate water-reducer, it is characterised in that:It is made of with the raw material of following weight proportions,
    18~26 parts of acrylic acid, 8~14 parts of thioacetic acid, 18~34 parts of isoamyl alcohol polyoxyethylene ether, 1~7 part of hydrogen peroxide, 1~7 part of vitamin C, 1~3 part of white sugar, 0.2~0.8 part of dodecyl sodium sulfate, 80~90 parts of solid naphthalene, the concentrated sulfuric acid 80~ 120 parts, 30~42 parts of formaldehyde, 30~40 parts of liquid caustic soda, 14~22 parts of polyethylene glycol monomethyl ethermethacrylic acid esters, lignin sulfonic acid 10~20 parts of calcium, 8~12 parts of ethylene oxide-propylene oxide copolymer, 1~3 part of trehalose, 1~2 part of silicone powder, shale ashes 2.5 ~6.5 parts, 1.5~3.5 parts of sodium hydrogensulfite, 4~8 parts of polyethylene glycol oxide, 6.5~10.5 parts of aluminium triphosphate, cocounut oil acyl two 2~4 parts of monoethanolamine, 0.5~1.5 part of dinonyl naphthalene sulfonate barium, 1~3 part of methenamine, 0.5~1.5 part of auxiliary agent, acetone 35~ 55 parts, 80~180 parts of sodium sulfite, 10~30 parts of acrylamide, 2~7 parts of initiator, 300~500 parts of water.
  2. A kind of 2. high performance polycarboxylate water-reducer according to claim 1, it is characterised in that:The auxiliary agent is with following The raw material of weight proportion is made,
    10~20 parts of magnesia, 4~8 parts of Humic acid Magnesium, 3~6 parts of ammonium benzoate, 9~15 parts of α-sodium olefin sulfonate, six phosphorus of inositol 2~4 parts of acid esters, 3~7 parts of isobutene triethoxysilane, 8~12 parts of poly-ferric chloride, 15~21 parts of germanite powder, titanium dioxide 8 ~12 parts, 1~3 part of myristyl glucoside, 6~9 parts of polyamide wax, 3~5 parts of lithium magnesium silicate, 1.5~4.5 parts of Tea Saponin.
  3. A kind of 3. high performance polycarboxylate water-reducer according to claim 1, it is characterised in that:The initiator is over cure Any one or more in hydrochlorate, including potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate.
  4. A kind of 4. preparation method of high performance polycarboxylate water-reducer as described in claim 1,2 or 3, it is characterised in that bag Include following steps:
    A, isoamyl alcohol polyoxyethylene ether is put into agitator tank with water and stirred evenly, obtain A product;
    B, at low ambient temperatures toward sequentially add in A product acrylic acid, thioacetic acid, hydrogen peroxide, vitamin C, liquid caustic soda, white sugar and Dodecyl sodium sulfate, is mixed, and obtains B product;
    C, B product are filtered and drying and processing, obtains C product;
    D, thawing processing is carried out to solid naphthalene, will be heated in solid naphthalene inputization naphthalene kettle, solid naphthalene is heated to melting at 80 DEG C Change, obtain D product;
    E, to D product carry out sulfonation processing, D product are positioned in sulphonation kettle with the concentrated sulfuric acid and are reacted, reacted in sulphonation kettle when Between be 3h, the temperature reacted in sulphonation kettle is 160~165 DEG C, obtains E product;
    F, cooling treatment is carried out to E product, is hydrolyzed after E product are cooled down, obtains F product;
    G, condensation processing is carried out to F product, F product is positioned in condensation kettle, formaldehyde is added in condensation kettle and is reacted, obtains G product;
    H, G product are neutralized, G product is positioned over and are neutralized in kettle, in and liquid caustic soda is added dropwise in kettle, obtains H product;
    I, H product are filtered and drying and processing, obtains I product;
    J, auxiliary agent is added into I product, stirs evenly, obtain J product;
    K, toward sequentially adding polyethylene glycol monomethyl ethermethacrylic acid esters, calcium lignosulfonate, ethylene oxide-epoxy third in J product Alkyl copolymer, trehalose, silicone powder, shale ashes, sodium hydrogensulfite, polyethylene glycol oxide, aluminium triphosphate, cocounut oil acyl diethanol Amine, dinonyl naphthalene sulfonate barium and methenamine, are mixed, and obtain K product;
    L, K product are filtered and pressure spray dryer is handled, obtain L product;
    M, acrylamide, sodium sulfite and water are positioned in reaction kettle, are warming up to 50~55 DEG C of dissolvings, then first is at the uniform velocity added dropwise Aldehyde, 1h are dripped off, then cooling discharging, obtain M product;
    N, water and sodium sulfite are positioned over stirring and dissolving in another reaction kettle, then acetone is added dropwise, add initiator, then first is added dropwise Aldehyde, is then added dropwise M product, finally adds water and cools down, obtains N product;
    O, N product are filtered and drying and processing, obtains O product;
    P, C product, L product and 0 product are stirred evenly, obtains finished product.
  5. 5. preparation method according to claim 4, it is characterised in that:Auxiliary agent in the step g passes through following steps system It is standby,
    A1, mixed magnesia, germanite powder, titanium dioxide, obtains A1 product;
    B1, toward sequentially adding α-sodium olefin sulfonate, isobutene triethoxysilane, polyamide wax and lithium magnesium silicate in A1 product, into Row mixing, obtains B1 product;
    B1 product, is positioned over 10~14min of stirring under 40~60 DEG C of bath temperatures by c1, is cooled to room temperature, is obtained C1 product;
    D1, toward sequentially adding Humic acid Magnesium, ammonium benzoate, inositol hexaphosphate, poly-ferric chloride, myristyl glucose in C1 product Glycosides and Tea Saponin stirring, are mixed, obtain finished product.
  6. 6. preparation method according to claim 4, it is characterised in that:Low temperature environment is 5~20 DEG C in the step b;Institute State in step f and E product are cooled down, E product is cooled to 120 DEG C and be hydrolyzed again, hydrolysis time 0.5h.
  7. 7. preparation method according to claim 4, it is characterised in that:In the step h in and in kettle during dropwise addition liquid caustic soda, Until when the pH value neutralized in kettle is located at 7~9, stop that liquid caustic soda is added dropwise;Pressure spray dryer processing is to utilize in the step l High-pressure pump, with the pressure of 150Mpa, by material by atomizer, the dimerization particulate that nebulizes directly is contacted with hot-air, carries out heat Exchange, the short time completes drying.
  8. 8. preparation method according to claim 4, it is characterised in that:In the step m when formaldehyde is added dropwise, process is added dropwise In temperature control at 68~72 DEG C, drip off follow-up continuation of insurance temperature 3h.
  9. 9. preparation method according to claim 4, it is characterised in that:It is to place water and sodium sulfite in the step n The stirring and dissolving in another reaction kettle, then acetone is at the uniform velocity added dropwise, 0.5h is dripped off;Initiator is added, then formaldehyde is at the uniform velocity added dropwise, 2h drops It is complete, while M product are added dropwise, and controlled at 90~95 DEG C, then keep the temperature 2h;Finally plus water and it is cooled to less than 40 DEG C, obtains N Product.
  10. 10. the preparation method according to any claim in claim 4 to 9, it is characterised in that:Dripped in the step g Add the number all same for being added dropwise in the number of formaldehyde, step m and formaldehyde being added dropwise in the number and step n of formaldehyde.
CN201711220624.4A 2017-11-29 2017-11-29 A kind of high performance polycarboxylate water-reducer and preparation method thereof Withdrawn CN107903565A (en)

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CN108569905A (en) * 2018-06-17 2018-09-25 刘玉清 A kind of ceramics liquefacient and preparation method thereof
CN110451843A (en) * 2019-08-03 2019-11-15 徐州巨龙新材料科技有限公司 A kind of high efficiency water reducing agent and preparation method thereof
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CN110482900A (en) * 2019-08-03 2019-11-22 徐州巨龙新材料科技有限公司 A kind of retardation setting type fatty family water-reducing agent and preparation method thereof
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CN115594467A (en) * 2022-11-21 2023-01-13 湖南大学(Cn) Self-leveling self-compacting wear-resistant floor material and preparation method thereof

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