CN108821630A - A kind of synthesis technology of low temperature polycarboxylate water-reducer - Google Patents
A kind of synthesis technology of low temperature polycarboxylate water-reducer Download PDFInfo
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- CN108821630A CN108821630A CN201810755467.5A CN201810755467A CN108821630A CN 108821630 A CN108821630 A CN 108821630A CN 201810755467 A CN201810755467 A CN 201810755467A CN 108821630 A CN108821630 A CN 108821630A
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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
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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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
- 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 a kind of synthesis technologies of low temperature polycarboxylate water-reducer, using the following raw material：Isobutene alcohol polyoxyethylene ether, polyoxyethylene ether, thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, methylpropene sodium sulfonate, liquid alkaline, organic amine, initiator, thioglycolic acid, low-temperature reduction agent, ascorbic acid, tartaric acid.The synthesis of present invention progress polycarboxylate water-reducer, reaction temperature can be effectively reduced, shorten the reaction time, and easy to operate, reaction process is more easily controlled, production efficiency improves high, production cost also has certain reduction, and the water-reducing agent adaptability of production is good, adapts to all kinds of cement substantially, a kind of new polymerization is provided for polycarboxylate water-reducer, there is research and application prospect well.
Description
Technical field
The present invention relates to water-reducing agent technical field, the synthesis technology of specifically a kind of low temperature polycarboxylate water-reducer.
Background technique
Water-reducing agent can be effectively improved the workability of concrete, improve the intensity of concrete, extend the durable of concrete
Property.During the higher concrete concentrated compactness of current the degree of automation, mechanical transport and pumping construction, water-reducing agent plays pole
Its important role, oneself is through becoming indispensable component in concrete.
According to the development process of water-reducing agent, the development of water-reducing agent is generally divided into three phases：The first generation is with calcium lignosulfonate, wood
Sodium is the ordinary water-reducing agent of representative, and water-reducing rate is in 6-12%；The second generation is using naphthalene system and melamine as the efficient diminishing of representative
There is the problems such as formaldehyde pollution in the production and use process in 15-25% in agent, water-reducing rate；The third generation is to be with polycarboxylate
The high-performance water reducing agent of representative has water-reducing rate high (up to 30%), and volume is few (0.2%-0.4%), institute's concrete batching tool
Have the advantages that intensity is high, environmentally protective, is the leading products and developing direction of additive industry from now on.
There are many approach of macromolecular synthetic reaction, can be divided into copolymerization, addition polymerization, polycondensation etc. according to reaction mechanism.Polycarboxylic acids
High-performance water reducing agent mainly passes through unsaturated monomer under the action of initiator, the active group with side chain is grafted to poly-
On the main chain for closing object, to obtain the polycarboxylate water-reducer molecule with pectinate texture.Currently, the synthesis temperature of polycarboxylate water-reducer
Degree is mostly at 80-120 DEG C, reaction time 3-8h.If polymerization technique can be improved, reaction is in low temperature and at room temperature, energy
The investment of boiler, cooling water recirculation system is saved, while simplifying technique, shortens the production cycle, reduces production cost, is improved economical
Benefit.
Summary of the invention
The purpose of the present invention is to provide a kind of low temperature polycarboxylate water-reducers for reducing reaction temperature, shortening the reaction time
Synthesis technology, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides the following technical solutions：
A kind of synthesis technology of low temperature polycarboxylate water-reducer, specific step is as follows：
(1) the following raw material is weighed according to parts by weight：30-50 parts of isobutene alcohol polyoxyethylene ether, polyoxyethylene ether 30-40
It is part, 20-40 parts of thioacetic acid, 5-10 parts of quaternary ammonium salt, 15-25 parts of acrylic acid, 5-10 parts of itaconic acid, 25-35 parts of chloroform, double
10-20 parts of oxygen water, 8-12 parts of methylpropene sodium sulfonate, 3-5 parts of liquid alkaline, 2-4 parts of organic amine, 1-2 parts of initiator, thioglycolic acid
0.5-1 parts, 1.5-2.5 parts of low-temperature reduction agent, 0.5-1 parts of ascorbic acid, 0.5-2.5 parts of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, Vitamin C
Acid, tartaric acid and 100-140 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 40-60 part water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 60-80 part water are added in reaction kettle, adjust reaction
Temperature is 5-30 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B are added dropwise simultaneously respectively, time for adding 2-4h, after completion of dropwise addition, disposably
It is added low-temperature reduction agent, the reaction was continued 1-2h is eventually adding the liquid alkaline that concentration is 25-35% and is neutralized to get to described
Polycarboxylate superplasticizer mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 8-12cm, is opened true
Sky pump adjusts the vacuum degree in drying box to -0.1~-0.06MPa；
(7) setting ultrasonic frequency is 30-50kHz, opens microwave generator, and microwave frequency is 915MHz or 2450MHz,
It is 30-50 DEG C that drying temperature, which is arranged, and adjusts range of microwave power to 100-300kW, dries 0.8-1.2h, obtains solid polycarboxylic acids
Water-reducing agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
As a further solution of the present invention：
The following raw material is weighed according to parts by weight in the step (1)：35-45 parts of isobutene alcohol polyoxyethylene ether, polyoxy second
32-38 parts of alkene ether, 25-35 parts of thioacetic acid, 6-9 parts of quaternary ammonium salt, 18-22 parts of acrylic acid, 6-9 parts of itaconic acid, chloroform 28-
32 parts, 12-18 parts of hydrogen peroxide, 9-11 parts of methylpropene sodium sulfonate, 3.5-4.5 parts of liquid alkaline, 2.5-3.5 parts of organic amine, initiator
1.2-1.8 parts, 0.6-0.9 parts of thioglycolic acid, 1.8-2.2 parts of low-temperature reduction agent, 0.6-0.9 parts of ascorbic acid, tartaric acid 1-2
Part.
As a further solution of the present invention：
The following raw material is weighed according to parts by weight in the step (1)：40 parts of isobutene alcohol polyoxyethylene ether, polyoxyethylene ether
35 parts, 30 parts of thioacetic acid, quaternary ammonium salt 8,20 parts of acrylic acid, 8 parts of itaconic acid, 30 parts of chloroform, 15 parts of hydrogen peroxide, methyl-prop
It is 10 parts of alkene sodium sulfonate, 4 parts of liquid alkaline, 3 parts of organic amine, 1.5 parts of initiator, 0.8 part of thioglycolic acid, 2 parts of low-temperature reduction agent, anti-bad
0.8 part of hematic acid, 1.5 parts of tartaric acid.
As a further solution of the present invention：
The organic amine is at least one of three hydroxypropylhydroxyethylcellulose ethylenediamines and tetrahydroxypropyl ethylenediamine.
As a further solution of the present invention：
The polyoxyethylene poly-oxygen propylene aether is isobutenyl polyoxyethylene poly-oxygen propylene aether and isopentene group polyoxyethylene
At least one of polyethenoxy ether, the molecular weight of the polyoxyethylene poly-oxygen propylene aether are 2200-3200.
As a further solution of the present invention：
The initiator is in azo-bis-iso-dimethyl, azodiisobutyronitrile and di-isopropyl peroxydicarbonate
It is at least one.
As further scheme of the invention：
The low-temperature reduction agent is 2- hydroxyl -2- sulfinatoacetic acid, 2- hydroxyl -2- sulfinatoacetic acid disodium salt, 2-
Hydroxyl -2- sulfonatoacetic acid or 2- hydroxyl -2- sulfonatoacetic acid disodium salt.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention carries out the synthesis of polycarboxylate water-reducer, can be effectively reduced reaction temperature, shortens the reaction time, and
Easy to operate, reaction process is more easily controlled, and production efficiency improves height, and production cost also has certain reduction, the diminishing of production
Agent adaptability is good, adapts to all kinds of cement substantially, provides a kind of new polymerization for polycarboxylate water-reducer, has and grind well
Study carefully and application prospect.
Specific embodiment
The technical solution of the patent is explained in further detail With reference to embodiment.
Embodiment 1
A kind of synthesis technology of low temperature polycarboxylate water-reducer, specific step is as follows：
(1) the following raw material is weighed according to parts by weight：30 parts of isobutene alcohol polyoxyethylene ether, 30 parts of polyoxyethylene ether, sulfydryl
20 parts of acetic acid, 5 parts of quaternary ammonium salt, 15 parts of acrylic acid, 5 parts of itaconic acid, 25 parts of chloroform, 10 parts of hydrogen peroxide, methacrylic sulfonic acid
8 parts of sodium, 3 parts of liquid alkaline, 2 parts of organic amine, 1 part of initiator, 0.5 part of thioglycolic acid, 1.5 parts of low-temperature reduction agent, ascorbic acid 0.5
Part, 0.5 part of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, Vitamin C
Acid, tartaric acid and 100 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 40 parts of water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 60 parts of water are added in reaction kettle, adjust reaction temperature
It is 5 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B is added dropwise simultaneously respectively, time for adding 2h is disposable to add after completion of dropwise addition
Enter low-temperature reduction agent, the reaction was continued 1h is eventually adding the liquid alkaline that concentration is 25% and is neutralized and subtracts to get to the polycarboxylic acids
Aqua mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 8cm, opens vacuum
Pump adjusts the vacuum degree in drying box to -0.1MPa；
(7) setting ultrasonic frequency is 30kHz, opens microwave generator, and drying temperature is arranged in microwave frequency 915MHz
It is 30 DEG C, and adjusts range of microwave power to 100kW, dries 0.8h, obtain solid polycarboxylic acid water reducing agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
Embodiment 2
A kind of synthesis technology of low temperature polycarboxylate water-reducer, specific step is as follows：
(1) the following raw material is weighed according to parts by weight：35 parts of isobutene alcohol polyoxyethylene ether, 32 parts of polyoxyethylene ether, sulfydryl
25 parts of acetic acid, 6 parts of quaternary ammonium salt, 18 parts of acrylic acid, 6 parts of itaconic acid, 28 parts of chloroform, 12 parts of hydrogen peroxide, methacrylic sulfonic acid
It is 9 parts of sodium, 3.5 parts of liquid alkaline, 2.5 parts of organic amine, 1.2 parts of initiator, 0.6 part of thioglycolic acid, 1.8 parts of low-temperature reduction agent, anti-bad
0.6 part of hematic acid, 1 part of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, Vitamin C
Acid, tartaric acid and 110 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 45 parts of water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 65 parts of water are added in reaction kettle, adjust reaction temperature
It is 10 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B is added dropwise simultaneously respectively, time for adding .5h is disposable to add after completion of dropwise addition
Enter low-temperature reduction agent, the reaction was continued 1.2h is eventually adding the liquid alkaline that concentration is 28% and is neutralized to get to the polycarboxylic acids
Water-reducing agent mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 9cm, opens vacuum
Pump adjusts the vacuum degree in drying box to -0.09MPa；
(7) setting ultrasonic frequency is 35kHz, opens microwave generator, and dry temperature is arranged in microwave frequency 2450MHz
Degree is 35 DEG C, and adjusts range of microwave power to 150kW, dries 0.9h, obtains solid polycarboxylic acid water reducing agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
Embodiment 3
A kind of synthesis technology of low temperature polycarboxylate water-reducer, specific step is as follows：
(1) the following raw material is weighed according to parts by weight：40 parts of isobutene alcohol polyoxyethylene ether, 35 parts of polyoxyethylene ether, sulfydryl
30 parts of acetic acid, quaternary ammonium salt 8,20 parts of acrylic acid, 8 parts of itaconic acid, 30 parts of chloroform, 15 parts of hydrogen peroxide, methylpropene sodium sulfonate
10 parts, 4 parts of liquid alkaline, 3 parts of organic amine, 1.5 parts of initiator, 0.8 part of thioglycolic acid, 2 parts of low-temperature reduction agent, ascorbic acid 0.8
Part, 1.5 parts of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, Vitamin C
Acid, tartaric acid and 120 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 50 parts of water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 70 parts of water are added in reaction kettle, adjust reaction temperature
It is 15 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B is added dropwise simultaneously respectively, time for adding 3h is disposable to add after completion of dropwise addition
Enter low-temperature reduction agent, the reaction was continued 1.5h is eventually adding the liquid alkaline that concentration is 30% and is neutralized to get to the polycarboxylic acids
Water-reducing agent mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 10cm, opens vacuum
Pump adjusts the vacuum degree in drying box to -0.08MPa；
(7) setting ultrasonic frequency is 40kHz, opens microwave generator, and drying temperature is arranged in microwave frequency 915MHz
It is 40 DEG C, and adjusts range of microwave power to 200kW, dries 1h, obtain solid polycarboxylic acid water reducing agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
Embodiment 4
A kind of synthesis technology of low temperature polycarboxylate water-reducer, specific step is as follows：
(1) the following raw material is weighed according to parts by weight：45 parts of isobutene alcohol polyoxyethylene ether, 38 parts of polyoxyethylene ether, sulfydryl
35 parts of acetic acid, 9 parts of quaternary ammonium salt, 22 parts of acrylic acid, 9 parts of itaconic acid, 32 parts of chloroform, 18 parts of hydrogen peroxide, methacrylic sulfonic acid
It is 11 parts of sodium, 4.5 parts of liquid alkaline, 3.5 parts of organic amine, 1.8 parts of initiator, 0.9 part of thioglycolic acid, 2.2 parts of low-temperature reduction agent, anti-bad
0.9 part of hematic acid, 2 parts of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, Vitamin C
Acid, tartaric acid and 130 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 55 parts of water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 75 parts of water are added in reaction kettle, adjust reaction temperature
It is 20 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B are added dropwise simultaneously respectively, time for adding .3.5h, after completion of dropwise addition, disposably
It is added low-temperature reduction agent, the reaction was continued 1.8h is eventually adding the liquid alkaline that concentration is 32% and is neutralized to get to the poly- carboxylic
Sour water-reducing agent mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 11cm, opens vacuum
Pump adjusts the vacuum degree in drying box to -0.07MPa；
(7) setting ultrasonic frequency is 45kHz, opens microwave generator, and dry temperature is arranged in microwave frequency 2450MHz
Degree is 45 DEG C, and adjusts range of microwave power to 250kW, dries 1.1h, obtains solid polycarboxylic acid water reducing agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
Embodiment 5
A kind of synthesis technology of low temperature polycarboxylate water-reducer, specific step is as follows：
(1) the following raw material is weighed according to parts by weight：50 parts of isobutene alcohol polyoxyethylene ether, 40 parts of polyoxyethylene ether, sulfydryl
40 parts of acetic acid, 10 parts of quaternary ammonium salt, 25 parts of acrylic acid, 10 parts of itaconic acid, 35 parts of chloroform, 20 parts of hydrogen peroxide, metering system sulphur
12 parts of sour sodium, 5 parts of liquid alkaline, 4 parts of organic amine, 2 parts of initiator, 1 part of thioglycolic acid, 2.5 parts of low-temperature reduction agent, ascorbic acid 1
Part, 2.5 parts of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, Vitamin C
Acid, tartaric acid and 140 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 60 parts of water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 80 parts of water are added in reaction kettle, adjust reaction temperature
It is 30 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B is added dropwise simultaneously respectively, time for adding 4h is disposable to add after completion of dropwise addition
Enter low-temperature reduction agent, the reaction was continued 2h is eventually adding the liquid alkaline that concentration is 35% and is neutralized and subtracts to get to the polycarboxylic acids
Aqua mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 12cm, opens vacuum
Pump adjusts the vacuum degree in drying box to -0.06MPa；
(7) setting ultrasonic frequency is 50kHz, opens microwave generator, and drying temperature is arranged in microwave frequency 915MHz
It is 50 DEG C, and adjusts range of microwave power to 300kW, dries 1.2h, obtain solid polycarboxylic acid water reducing agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
The organic amine is at least one of three hydroxypropylhydroxyethylcellulose ethylenediamines and tetrahydroxypropyl ethylenediamine.The polyoxy
Ethylene polyethenoxy ether be in isobutenyl polyoxyethylene poly-oxygen propylene aether and isopentene group polyoxyethylene poly-oxygen propylene aether extremely
Few one kind, the molecular weight of the polyoxyethylene poly-oxygen propylene aether are 2200-3200.The initiator is two isobutyric acid diformazan of azo
At least one of ester, azodiisobutyronitrile and di-isopropyl peroxydicarbonate.The low-temperature reduction agent is 2- hydroxyl -2- sub-
Sulfonatoacetic acid, 2- hydroxyl -2- sulfinatoacetic acid disodium salt, 2- hydroxyl -2- sulfonatoacetic acid or 2- hydroxyl -2- sulfonic group second
Acid disodium salt.
The present invention carries out the synthesis of polycarboxylate water-reducer, can be effectively reduced reaction temperature, shortens the reaction time, and
Easy to operate, reaction process is more easily controlled, and production efficiency improves height, and production cost also has certain reduction, the diminishing of production
Agent adaptability is good, adapts to all kinds of cement substantially, provides a kind of new polymerization for polycarboxylate water-reducer, has and grind well
Study carefully and application prospect.
The preferred embodiment of the patent is described in detail above, but this patent is not limited to above-mentioned embodiment party
Formula within the knowledge of one of ordinary skill in the art can also be under the premise of not departing from this patent objective
Various changes can be made.
Claims (7)
1. a kind of synthesis technology of low temperature polycarboxylate water-reducer, which is characterized in that specific step is as follows：
(1) the following raw material is weighed according to parts by weight：30-50 parts of isobutene alcohol polyoxyethylene ether, 30-40 parts of polyoxyethylene ether, mercapto
20-40 parts of guanidine-acetic acid, 5-10 parts of quaternary ammonium salt, 15-25 parts of acrylic acid, 5-10 parts of itaconic acid, 25-35 parts of chloroform, hydrogen peroxide
10-20 parts, 8-12 parts of methylpropene sodium sulfonate, 3-5 parts of liquid alkaline, 2-4 parts of organic amine, 1-2 parts of initiator, thioglycolic acid 0.5-
1 part, 1.5-2.5 parts of low-temperature reduction agent, 0.5-1 parts of ascorbic acid, 0.5-2.5 parts of tartaric acid；
(2) by thioacetic acid, quaternary ammonium salt, acrylic acid, itaconic acid, chloroform, hydrogen peroxide, thioglycolic acid, ascorbic acid, wine
Stone acid and 100-140 parts of water are configured to mixed solution A；
(3) methylpropene sodium sulfonate, organic amine and 40-60 part water are configured to mixed solution B；
(4) isobutene alcohol polyoxyethylene ether, polyoxyethylene ether and 60-80 part water are added in reaction kettle, adjust reaction temperature
It is 5-30 DEG C, is added at one time initiator, stirs to dissolve；
(5) mixed solution A and mixed solution B is added dropwise simultaneously respectively, time for adding 2-4h after completion of dropwise addition, is added at one time
Low-temperature reduction agent, the reaction was continued 1-2h are eventually adding the liquid alkaline that concentration is 25-35% and are neutralized to get to the poly- carboxylic
Sour water-reducing agent mother liquor；
(6) polycarboxylate superplasticizer mother liquor is placed in vacuum ultrasonic microwave drying oven, mother liquor depth is 8-12cm, opens vacuum pump
The vacuum degree in drying box is adjusted to -0.1~-0.06MPa；
(7) setting ultrasonic frequency is 30-50kHz, opens microwave generator, and microwave frequency is 915MHz or 2450MHz, setting
Drying temperature is 30-50 DEG C, and adjusts range of microwave power to 100-300kW, dries 0.8-1.2h, obtains solid polycarboxylic acids diminishing
Agent；
(8) solid polycarboxylic acid water reducing agent that step (7) is dried to obtain is grinding to obtain polycarboxylate water-reducer pulvis.
2. the synthesis technology of low temperature polycarboxylate water-reducer according to claim 1, which is characterized in that in the step (1)
The following raw material is weighed according to parts by weight：35-45 parts of isobutene alcohol polyoxyethylene ether, 32-38 parts of polyoxyethylene ether, thioacetic acid
25-35 parts, 6-9 parts of quaternary ammonium salt, 18-22 parts of acrylic acid, 6-9 parts of itaconic acid, 28-32 parts of chloroform, 12-18 parts of hydrogen peroxide,
9-11 parts of methylpropene sodium sulfonate, 3.5-4.5 parts of liquid alkaline, 2.5-3.5 parts of organic amine, 1.2-1.8 parts of initiator, thioglycolic acid
0.6-0.9 parts, 1.8-2.2 parts of low-temperature reduction agent, 0.6-0.9 parts of ascorbic acid, 1-2 parts of tartaric acid.
3. the synthesis technology of low temperature polycarboxylate water-reducer according to claim 1, which is characterized in that in the step (1)
The following raw material is weighed according to parts by weight：40 parts of isobutene alcohol polyoxyethylene ether, 35 parts of polyoxyethylene ether, 30 parts of thioacetic acid, season
Ammonium salt 8,20 parts of acrylic acid, 8 parts of itaconic acid, 30 parts of chloroform, 15 parts of hydrogen peroxide, 10 parts of methylpropene sodium sulfonate, liquid alkaline 4
Part, 3 parts of organic amine, 1.5 parts of initiator, 0.8 part of thioglycolic acid, 2 parts of low-temperature reduction agent, 0.8 part of ascorbic acid, tartaric acid
1.5 part.
4. the synthesis technology of low temperature polycarboxylate water-reducer according to claim 1 to 3, which is characterized in that described organic
Amine is at least one of three hydroxypropylhydroxyethylcellulose ethylenediamines and tetrahydroxypropyl ethylenediamine.
5. the synthesis technology of low temperature polycarboxylate water-reducer according to claim 1 to 3, which is characterized in that the polyoxy
Ethylene polyethenoxy ether be in isobutenyl polyoxyethylene poly-oxygen propylene aether and isopentene group polyoxyethylene poly-oxygen propylene aether extremely
Few one kind, the molecular weight of the polyoxyethylene poly-oxygen propylene aether are 2200-3200.
6. the synthesis technology of low temperature polycarboxylate water-reducer according to claim 1 to 3, which is characterized in that the initiation
Agent is at least one of azo-bis-iso-dimethyl, azodiisobutyronitrile and di-isopropyl peroxydicarbonate.
7. the synthesis technology of low temperature polycarboxylate water-reducer according to claim 1 to 3, which is characterized in that the low temperature
Reducing agent is 2- hydroxyl -2- sulfinatoacetic acid, 2- hydroxyl -2- sulfinatoacetic acid disodium salt, 2- hydroxyl -2- sulfonatoacetic acid
Or 2- hydroxyl -2- sulfonatoacetic acid disodium salt.
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| CN111592264A (en) * | 2020-05-26 | 2020-08-28 | 重庆三圣实业股份有限公司 | Dicarboxyl sulfonic acid group polycarboxylic acid water reducing agent and preparation method thereof |
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Application publication date: 20181116 |