CN111040081B - Preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance - Google Patents
Preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance Download PDFInfo
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- CN111040081B CN111040081B CN202010037861.2A CN202010037861A CN111040081B CN 111040081 B CN111040081 B CN 111040081B CN 202010037861 A CN202010037861 A CN 202010037861A CN 111040081 B CN111040081 B CN 111040081B
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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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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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
- C04B24/38—Polysaccharides or derivatives thereof
- C04B24/383—Cellulose or derivatives thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to the technical field of modified synthesis of cellulose ether, and particularly discloses a preparation method of high-suspension, strong-rheology and bleeding-prevention cellulose ether, which comprises the following steps: the invention makes the cellulose ether have the advantages of high water-retaining property, low viscosity, high suspension, strong rheology, anti-settling and the like, is used in mortar such as self-leveling mortar, grouting material, grouting agent, high-performance concrete and the like, can ensure high fluidity and pumping property, simultaneously avoids the phenomena of sand setting, bleeding, layering, segregation and the like during construction, keeps the cohesive viscosity of pouring self-leveling mortar, grouting material and concrete, ensures the uniformity and stability of the hardened mortar, and avoids the quality problem.
Description
Technical Field
The invention belongs to the technical field of modified synthesis of cellulose ether, and particularly relates to a preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance.
Background
In mortar and concrete, cellulose ether is used as an indispensable additive, and is widely applied to mortar and concrete by virtue of excellent water retention and thickening performance, the cellulose ether can play a role in water retention and thickening in the mortar and concrete, can also prevent mortar from segregating, settling and bleeding, and improves the workability and the workability of the mortar, and for products with higher requirements on fluidity, such as self-leveling, grouting materials, grouting agents, high-performance concrete and the like, the cellulose ether with lower viscosity is used, but the products such as self-leveling, grouting materials, grouting agents, high-performance concrete and the like often cause the sinking of coarse aggregate, the floating of fine materials, segregating and bleeding, upper and lower layering, and the surface strength pulverization after the cement is hardened, the problem of inconsistent surface layer and internal strength, the product performance is seriously reduced, the strength, the stability and the durability of the mortar, particularly the concrete are influenced, and great potential safety hazards are caused to the engineering quality; at present, the low-viscosity cellulose ether has too low viscosity and limited thickening effect, and can not effectively improve the problem, while the high-viscosity cellulose ether has obvious thickening effect, but can cause the self-leveling, grouting material, grouting agent and high-performance concrete to be immobile due to overlarge viscosity, and the pumping property and the leveling property of the high-viscosity cellulose ether are influenced, so that the low-viscosity cellulose ether is subjected to rheological modification to improve the problems of sand setting, bleeding, layering and the like existing in the self-leveling and grouting material, so that the high-flow mortar and the high-performance concrete can have excellent flow property, can not be isolated and settled, and the quality problem generated in the using process is avoided to be urgently needed to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of high-suspension, strong-rheology and bleeding-prevention cellulose ether, which ensures that low-viscosity cellulose ether has excellent suspension, thixotropic and anti-settling properties while keeping conventional water retention and thickening properties, brings excellent workability and stability for products with high flow property requirements such as self-leveling, grouting materials, grouting agents, high-performance concrete and the like, perfectly solves the problems of sand setting, bleeding, layering and the like during construction, and avoids the problem of engineering quality.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance comprises the following steps:
(1) Preparing cellulose ether with viscosity of 400-1000mpa.s: soaking refined cotton in 40% NaOH solution for 1h, then carrying out alkalization treatment at 30 ℃, sealing and vacuumizing a reaction kettle, and adding an etherifying agent, wherein the mass ratio of cotton fibers to the etherifying agent is 1:1.5-2.0, slowly heating to 40 ℃ for reaction for 2 hours, and continuously heating to 70 ℃ for reaction for 1.5 hours to obtain the catalyst;
(2) Carrying out modification substitution treatment on the cellulose ether prepared in the step (1): putting the cellulose ether prepared in the step (1) into a reaction kettle, quickly heating the reaction kettle to 80 ℃, adding a water-soluble rheological polymerization modified monomer into the reaction kettle, then adding an initiator and a catalyst, wherein the adding amounts of the initiator and the catalyst are respectively 1% and 2% of the mass of the cellulose ether, stirring at a low speed of 60r/min, and fully reacting for 2 hours to obtain the modified cellulose ether.
Further, the cellulose ether prepared in the step (1) is at least one of hydroxypropyl methyl cellulose ether or hydroxyethyl methyl cellulose ether, and the etherifying agent is one of methyl chloride, propylene oxide, methyl chloride and ethylene oxide.
Further, the mass ratio of the cellulose ether to the water-soluble rheological polymerization modification monomer in the step (2) is 1-3:1.
further, the water-soluble rheological polymerization modified monomer in the step (2) is an organic polymer monomer, the organic polymer monomer is at least one of an ethylene oxide monomer, an acrylamide monomer, a vinylpyrrolidone monomer, an acryloyl dimethyl taurine monomer and a methyl acrylate sodium sulfonate monomer, the initiator is at least one of potassium persulfate or sodium persulfate, and the catalyst is at least one of antimony dioxide or ferric trichloride.
The reaction mechanism of the invention is as follows: the dispersibility and the solubility of the cellulose ether substituted by the ethylene oxide monomer and the acrylamide monomer are greatly improved, the thickening property, the suspension property and the stability are improved, the monomer with rheological property forms low-viscosity sol when the concentration is low after polymerization reaction, the sol is close to Newtonian fluid, the concentration is increased to form high-viscosity sol, the sol is non-Newtonian fluid, after the shearing force is applied, the network is destroyed, and after the shearing force is eliminated, the network can be quickly recovered, so that the thickening, thixotropic and anti-sedimentation effects are achieved, and after the polymerization substitution reaction, molecules are uniformly isolated and dispersed in a space matrix-like mode through bridging and recombination, so that the segregation resistance and the bleeding resistance are improved.
The invention has the advantages that: aiming at the problem that the low-viscosity cellulose ether can not effectively solve the problems of sand setting, bleeding, layering and the like in self-leveling, grouting materials, grouting agents and high-performance concrete, the low-viscosity cellulose ether is modified, so that the low-viscosity cellulose ether has excellent suspension, thixotropy and anti-settling properties while keeping the characteristics of conventional water retention and thickening properties, brings excellent constructability and stability to products with high requirements on flow properties such as self-leveling, grouting materials, grouting agents and high-performance concrete, perfectly solves the problems of sand setting, bleeding, layering and the like during construction, and avoids the problem of engineering quality.
Detailed Description
Example 1
A preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance comprises the following steps:
(1) Preparing a cellulose ether having a viscosity of 400-1000mpa.s: soaking refined cotton in 40% NaOH solution for 1h, alkalizing at 30 deg.C, vacuumizing the reaction kettle, adding certain amount of etherifying agent which is one of methyl chloride, propylene oxide, methyl chloride and ethylene oxide, wherein the mass ratio of cotton fiber to etherifying agent is 1:1.5-2.0, slowly heating to 40 ℃ for reaction for 2h, and continuously heating to 70 ℃ for reaction for 1.5h to obtain the cellulose ether, wherein the prepared cellulose ether is at least one of hydroxypropyl methyl cellulose ether or hydroxyethyl methyl cellulose ether, and the initiator is at least one of potassium persulfate or sodium persulfate;
(2) Carrying out modification substitution treatment on the cellulose ether prepared in the step (1): putting the cellulose ether prepared in the step (1) into a reaction kettle, quickly heating the reaction kettle to 80 ℃, and adding a water-soluble rheological polymerization modified monomer into the reaction kettle, wherein the water-soluble rheological polymerization modified monomer is prepared by mixing and substituting an ethylene oxide monomer and an acrylamide monomer 1, and the mass ratio of the cellulose ether to the water-soluble rheological polymerization modified monomer is 1:1, adding an initiator and a catalyst, wherein the adding amount of the initiator and the catalyst is 1% and 2% of the cellulose ether respectively, stirring at a low speed of 60r/min, fully reacting for 2 hours to obtain the modified cellulose ether, and the viscosity of the prepared cellulose is 420mpa.s.
Example 2
Example 2 differs from example 1 in that: when the rheology modification treatment is carried out, the proportion of each component is approximately that the mass ratio of the cellulose ether to the water-soluble rheology polymerization modification monomer is 2.
Example 3
Example 3 differs from example 1 in that: when the rheology modification treatment is carried out, the proportion of each component is approximately that the mass ratio of the cellulose ether to the water-soluble rheology polymerization modification monomer is 3.
Example 4
Example 4 differs from example 1 in that: when the rheology modification treatment is carried out, the proportion of each component is approximately that the mass ratio of the cellulose ether to the water-soluble rheology polymerization modification monomer is 1, wherein the water-soluble rheology polymerization modification monomer is prepared by mixing and substituting ethylene oxide monomer and acrylamide monomer 3.
Application and comparison
The cellulose ethers prepared in examples 1 to 4 were used in self-leveling cements, the formulation of which is shown in table 1.
TABLE 1
A group of unmodified low-viscosity cellulose ethers is added into the self-leveling cement described in the table 1 to serve as a control group, the cellulose ethers prepared in the examples 1 to 4 are applied to the self-leveling cement, and the modified cellulose ethers are compared and tested on the self-leveling performance, mainly the influence of the fluidity, the bleeding sand setting condition and the strength according to the selection performance of a JC/985-2005 standard test, see table 2
| Unmodified low Viscosity fiber Sulfoxanthin ethers | Example 1 modified Low viscosity Cellulose ether | Example 2 modified Low viscosity Cellulose ether | Example 3 modified Low viscosity Cellulose ether | Example 4 modified Low viscosity Cellulose ether | JC/985-2005 Standard requirements of | |
| Amount of added water | 26% | 26% | 26% | 26% | 26% | - |
| Initial fluidity/mm | 140 | 145 | 146 | 142 | 146 | ≧130 |
| 30min fluidity/mm | 133 | 140 | 143 | 140 | 139 | ≧130 |
| Whether it secretes after 5min Water and sand setting | Bleeding and sand setting Severe severity of disease | No sand setting and no bleeding | No sand setting and no bleeding | No sand setting and no bleeding | No sand setting and no bleeding | No bleeding and sand setting |
| Abrasion value/g | 2.53 | 0.22 | 0.31 | 0.22 | 0.30 | ≤0.5 |
| 28d antiflex strength Mpa | 5.2 | 6.5 | 7.0 | 6.8 | 6.6 | ≧6.0 |
| 28d compressive strength- Mpa | 22.3 | 26.2 | 25.8 | 26.0 | 26.4 | ≧25 |
| 28d bonding strength Mpa | 0.85 | 1.18 | 1.14 | 1.09 | 1.17 | ≧1.0 |
Table 2.
Claims (2)
1. A preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance is characterized by comprising the following steps:
(1) Preparing cellulose ether with viscosity of 400-1000mpa.s: soaking refined cotton in 40% NaOH solution for 1h, then carrying out alkalization treatment at 30 ℃, sealing and vacuumizing a reaction kettle, and adding an etherifying agent, wherein the mass ratio of cotton fibers to the etherifying agent is 1:1.5-2.0, heating to 40 ℃ for reaction for 2h, and continuously heating to 70 ℃ for reaction for 1.5h to obtain the product;
(2) Carrying out modification substitution treatment on the cellulose ether prepared in the step (1): putting the cellulose ether prepared in the step (1) into a reaction kettle, heating the reaction kettle to 80 ℃, adding a water-soluble rheological polymerization modified monomer into the reaction kettle, then adding an initiator and a catalyst, wherein the adding amounts of the initiator and the catalyst are respectively 1% and 2% of the amount of the cellulose ether, stirring at a low speed of 60r/min, and fully reacting for 2 hours to obtain modified cellulose ether; the water-soluble rheological polymerization modified monomer is an ethylene oxide monomer and an acrylamide monomer, the initiator is at least one of potassium persulfate or sodium persulfate, and the catalyst is at least one of antimony dioxide or ferric trichloride; the mass ratio of the cellulose ether to the water-soluble rheological polymerization modified monomer is 1-3:1.
2. a process for preparing a highly suspended, high rheology, bleed resistant cellulose ether of claim 1 comprising: the cellulose ether prepared in the step (1) is at least one of hydroxypropyl methyl cellulose ether or hydroxyethyl methyl cellulose ether, and the etherifying agent is one of propylene oxide and ethylene oxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010037861.2A CN111040081B (en) | 2020-01-14 | 2020-01-14 | Preparation method of cellulose ether with high suspension, strong rheology and bleeding resistance |
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Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007261920A (en) * | 2006-03-30 | 2007-10-11 | Dainippon Ink & Chem Inc | Cement composition |
| BR112013018034B1 (en) * | 2011-12-01 | 2021-10-26 | Nutrition & Biosciences Usa 1, Llc | CONSTRUCTION COMPOSITION, METHOD FOR APPLYING A COMPOSITION FOR THE CONSTRUCTION AND USE OF A CELLULOSE ETHER |
| CN102515611B (en) * | 2011-12-13 | 2013-09-25 | 江南大学 | Multifunctional dry-mixed mortar additive and preparation method thereof |
| BR112015021081A2 (en) * | 2013-03-13 | 2020-01-28 | Akzo Nobel Chemicals Int Bv | polysaccharide alkali swellable rheology modifier; method of making polysaccharide alkaline swellable rheology modifier; and use of rheology modifier |
| CN105505253B (en) * | 2016-01-15 | 2018-07-10 | 上海惠广精细化工有限公司 | The preparation method of the dedicated modified hydroxypropyl methyl cellulose of technical grade ceramic tile series |
| CN105646950B (en) * | 2016-01-15 | 2019-01-29 | 上海惠广精细化工有限公司 | The preparation method of the dedicated modified hydroxypropyl methyl cellulose of technical grade thermal insulation mortar series |
| CN105542018B (en) * | 2016-01-15 | 2018-06-26 | 上海惠广精细化工有限公司 | The preparation method of the dedicated modified hydroxypropyl methyl cellulose of technical grade inner wall putty series |
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