CN110156935A - A kind of polymeric polycarboxylic acid dipersant preparation method - Google Patents
A kind of polymeric polycarboxylic acid dipersant preparation method Download PDFInfo
- Publication number
- CN110156935A CN110156935A CN201910421643.6A CN201910421643A CN110156935A CN 110156935 A CN110156935 A CN 110156935A CN 201910421643 A CN201910421643 A CN 201910421643A CN 110156935 A CN110156935 A CN 110156935A
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- CN
- China
- Prior art keywords
- preparation
- polycarboxylic acid
- polymeric polycarboxylic
- dipersant
- acid dipersant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- 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
- C08F283/065—Macromolecular 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
-
- 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 polymeric polycarboxylic acid dipersant preparation methods, used in invention the degree of polymerization for 60~90 high polymer monomer, as the side chain in polycarboxylate structure, make side chain that there is biggish length, form stronger steric hindrance effect, so the polycarboxylate water-reducer has good dispersion performance, and material is easy to get, it is at low cost, nontoxic byproduct, it directly synthesizes in a kettle, suitable for industrialized production, pass through the addition of zirconia balls, the heat that polymerization reaction is released mixes transmitting, facilitate control reaction temperature, it can be improved final product quality.
Description
Technical field
The present invention relates to dispersing agent field, specifically a kind of polymeric polycarboxylic acid dipersant preparation method.
Background technique
Dispersing agent is one kind in the molecule while having lipophilic and two kinds of opposite natures of hydrophily interfacial agent.It can
Those are poorly soluble in the inorganic of liquid, the solid particle of organic pigment for uniform dispersion, while can also prevent the heavy of solid particle
Drop and cohesion, medicament needed for forming stable suspension.Its mechanism of action: 1. are adsorbed in the surface of solid particle, make cohesion
Solid particles surface is easy to wet；2. the dispersing agent of polymer electrolyte forms adsorption layer on the surface of solid particle, makes solid particle
The charge on surface increases, and improves the intergranular reaction force for forming steric hindrance；3. solid particle surfaces is made to form bimolecular
Layer structure, outer layer dispersing agent polar end and water, which have, increases the degree solid particle that solids are spontaneously wet out by water compared with strong affinity
Between it is separate because of electrostatic repulsion；4. keeping system uniform, suspendability increases, and does not precipitate, keeps whole system physico-chemical property the same,
Existing polycarboxylic acid salt's dispersing agent generallys use polymerisation in solution when preparing, and polymerization reaction can give out amount of heat and to react
Temperature is difficult to control.
Summary of the invention
The purpose of the present invention is to provide a kind of polymeric polycarboxylic acid dipersant preparation methods, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the invention provides the following technical scheme: a kind of polymeric polycarboxylic acid dipersant preparation side
Method, comprising the following steps:
S1, by hydramine substance and unsaturated carboxylic acid difference it is soluble in water, be made mass concentration be 32-40% aqueous solution
It is spare；
S2, high polymer monomer is dissolved in distilled water, 20-30 DEG C of water-bath heating, and stirred, mass concentration, which is made, is
The aqueous solution of 32-40% is spare；
S3, initiator is dissolved in distilled water, it is spare that the aqueous solution that mass concentration is 32-40% is made；
S4, it will be stirred in the addition reaction kettle of aqueous solution made from S1, heating water bath is reaction 1-2 small to 70-80 DEG C
When；
S5, the reaction kettle in S4 is heated up, when temperature is promoted to 85-90 DEG C, will be made in S2 and S3 using peristaltic pump
Aqueous solution be gradually added dropwise in reaction kettle, it is lasting to stir, keep the temperature 4-5 hour of polymerization reaction；
S6, the copolymer solution for reacting completion in S5 is cooled to room temperature, neutralizer is added and adjusts, so that copolymer solution
PH value be 7；
S7, polycarboxylate salt dispersant will be obtained after the spray drying of copolymer solution made from S6.
As a further solution of the present invention: the hydramine substance is monoethanolamine, diethanol amine or triisopropanolamine
One of；
As a further solution of the present invention: the unsaturated carboxylic acid is one of maleic acid or methacrylic acid；
As a further solution of the present invention: the high polymer monomer is the allyl polyoxy second that the degree of polymerization is 60~90
One of which in alkene ether monomer, methylallyl alcohol polyoxyethylene ether monomer or methyl butenol polyoxyethylene ether monomer；
As a further solution of the present invention: as a further solution of the present invention: the initiator is ammonium persulfate, mistake
One of potassium sulfate or sodium peroxydisulfate；
As a further solution of the present invention: the quality proportioning high polymer monomer of each component: unsaturated carboxylic acid:
Hydramine substance: initiator is 1:0.1~0.15:0.002~0.015:0.003~0.020；
As a further solution of the present invention: the neutralizer is the sodium hydroxide solution of mass fraction 30%；
As a further solution of the present invention: several zirconia balls burnt by force, energy are placed in the reaction kettle
Enough while improving mixing effect, the heat mixing transmitting of polymerization reaction releasing is prevented office by the temperature in balanced reaction kettle
Portion's overheat.
Compared with prior art, the beneficial effects of the present invention are: used in invention the degree of polymerization for 60~90 macromolecule list
Body makes side chain have biggish length as the side chain in polycarboxylate structure, forms stronger steric hindrance effect, so
The polycarboxylate water-reducer has good dispersion performance, and material is easy to get, at low cost, nontoxic byproduct, in a kettle directly
Synthesis is suitable for industrialized production, and by the addition of zirconia balls, the heat that polymerization reaction is released mixes transmitting, convenient
Reaction temperature is controlled, can be improved final product quality.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
In the embodiment of the present invention, a kind of polymeric polycarboxylic acid dipersant preparation method, comprising the following steps:
S1, by hydramine substance and unsaturated carboxylic acid difference it is soluble in water, be made mass concentration be 32-40% aqueous solution
It is spare；
S2, high polymer monomer is dissolved in distilled water, 20-30 DEG C of water-bath heating, and stirred, mass concentration, which is made, is
The aqueous solution of 32-40% is spare；
S3, initiator is dissolved in distilled water, it is spare that the aqueous solution that mass concentration is 32-40% is made；
S4, it will be stirred in the addition reaction kettle of aqueous solution made from S1, heating water bath is reaction 1-2 small to 70-80 DEG C
When；
S5, the reaction kettle in S4 is heated up, when temperature is promoted to 85-90 DEG C, will be made in S2 and S3 using peristaltic pump
Aqueous solution be gradually added dropwise in reaction kettle, it is lasting to stir, keep the temperature 4-5 hour of polymerization reaction；
S6, the copolymer solution for reacting completion in S5 is cooled to room temperature, neutralizer is added and adjusts, so that copolymer solution
PH value be 7；
S7, polycarboxylate salt dispersant will be obtained after the spray drying of copolymer solution made from S6.
The hydramine substance is one of monoethanolamine, diethanol amine or triisopropanolamine；
The unsaturated carboxylic acid is one of maleic acid or methacrylic acid；
The high polymer monomer be the degree of polymerization be 60~90 allyl polyethenoxy ether monomer, methylallyl alcohol polyoxy
One of which in vinyl ether monomers or methyl butenol polyoxyethylene ether monomer；
The initiator is one of ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate；
The quality proportioning high polymer monomer of each component: unsaturated carboxylic acid: hydramine substance: initiator 1:
0.1~0.15:0.002~0.015:0.003~0.020；
The neutralizer is the sodium hydroxide solution of mass fraction 30%；
Several zirconia balls for burning by force are placed in the reaction kettle, can while improving mixing effect,
Temperature in balanced reaction kettle, the heat that polymerization reaction is released mix transmitting, prevent hot-spot.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of polymeric polycarboxylic acid dipersant preparation method, which comprises the following steps:
S1, by hydramine substance and unsaturated carboxylic acid difference it is soluble in water, be made mass concentration be 32-40% aqueous solution it is standby
With；
S2, high polymer monomer is dissolved in distilled water, 20-30 DEG C of water-bath heating, and stirred, it is 32- that mass concentration, which is made,
40% aqueous solution is spare；
S3, initiator is dissolved in distilled water, it is spare that the aqueous solution that mass concentration is 32-40% is made；
S4, it will be stirred in the addition reaction kettle of aqueous solution made from S1, heating water bath reacts 1-2 hour to 70-80 DEG C；
S5, the reaction kettle in S4 is heated up, when temperature is promoted to 85-90 DEG C, using peristaltic pump by water obtained in S2 and S3
Solution is gradually added dropwise in reaction kettle, lasting to stir, and keeps the temperature 4-5 hour of polymerization reaction；
S6, the copolymer solution for reacting completion in S5 is cooled to room temperature, neutralizer is added and adjusts, so that the PH of copolymer solution
Value is 7；
S7, polycarboxylate salt dispersant will be obtained after the spray drying of copolymer solution made from S6.
2. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that the hydramine
Substance is one of monoethanolamine, diethanol amine or triisopropanolamine.
3. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that the insatiable hunger
It is one of maleic acid or methacrylic acid with carboxylic acid.
4. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that the high score
Sub- monomer is allyl polyethenoxy ether monomer, methylallyl alcohol polyoxyethylene ether monomer or the methyl that the degree of polymerization is 60~90
One of which in butenol polyoxyethylene ether monomer.
5. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that the initiation
Agent is one of ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate.
6. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that each group
At the quality proportioning high polymer monomer of substance: unsaturated carboxylic acid: hydramine substance: initiator be 1:0.1~0.15:0.002~
0.015:0.003~0.020.
7. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that the neutralization
Agent is the sodium hydroxide solution of mass fraction 30%.
8. a kind of polymeric polycarboxylic acid dipersant preparation method according to claim 1, which is characterized in that the reaction
Several zirconia balls burnt by force are placed in kettle.
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| CN201910421643.6A CN110156935A (en) | 2019-05-21 | 2019-05-21 | A kind of polymeric polycarboxylic acid dipersant preparation method |
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| CN201910421643.6A CN110156935A (en) | 2019-05-21 | 2019-05-21 | A kind of polymeric polycarboxylic acid dipersant preparation method |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838313A (en) * | 2011-06-24 | 2012-12-26 | 魏中原 | Polycarboxylic acid series high molecular synthetic cement grinding additive and preparation method thereof |
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2019
- 2019-05-21 CN CN201910421643.6A patent/CN110156935A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838313A (en) * | 2011-06-24 | 2012-12-26 | 魏中原 | Polycarboxylic acid series high molecular synthetic cement grinding additive and preparation method thereof |
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Application publication date: 20190823 |
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