CN114890706A - Low-cost high-efficiency chlorine-free cement grinding aid and preparation method thereof - Google Patents
Low-cost high-efficiency chlorine-free cement grinding aid and preparation method thereof Download PDFInfo
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- CN114890706A CN114890706A CN202210391627.9A CN202210391627A CN114890706A CN 114890706 A CN114890706 A CN 114890706A CN 202210391627 A CN202210391627 A CN 202210391627A CN 114890706 A CN114890706 A CN 114890706A
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
- C04B24/122—Hydroxy amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/10—Separation; Purification; Stabilisation; Use of additives
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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
- C04B2103/52—Grinding aids; Additives added during grinding
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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
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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Abstract
The invention discloses a low-cost high-efficiency chlorine-free cement grinding aid which comprises the following components in parts by mass: 15-20 parts of a composite reinforcing agent II; 8-10 parts of sodium acetate; 12-15 parts of molasses. Meanwhile, the preparation method of the low-cost and high-efficiency chlorine-free cement grinding aid comprises the following steps: s1, preparing a composite reinforcing agent type II; s2, adding molasses and a composite reinforcing agent type II into a reaction vessel, and stirring and mixing uniformly to form a premix; s3, adding sodium acetate into the premix, stirring and mixing uniformly, and adding water until the sodium acetate is completely dissolved. The molasses and the composite reinforcer II are mixed firstly, and then the sodium acetate is added, so that the components are favorably and cooperatively matched with each other, the grinding aid effect of the grinding aid is favorably improved, the grinding efficiency of cement aggregates is higher, and the reduction of the screen residue of cement is favorably realized; expensive raw materials such as triethanolamine, triisopropanolamine, diethanolisopropanolamine and the like are not added in the prepared grinding aid, so that the cost of the grinding aid is greatly reduced.
Description
Technical Field
The invention relates to the technical field of cement production, in particular to a low-cost high-efficiency chlorine-free cement grinding aid and a preparation method thereof.
Background
At present, two major problems exist in cement production in China: firstly, the product quality is generally lower than foreign, secondly, the energy utilization rate is low, and the power consumption is high. The energy consumption of the cement mill has a great influence on the quality of finished products: on one hand, the fineness of the cement powder grinding, the particle composition and the particle shape play a great role in fully exerting the cement activity and improving the cement concrete performance; on the other hand, the fineness of the cement is improved, the performance of the cement is improved, the yield of the mill is reduced, the power consumption is increased, and the grinding process is the process with highest power consumption and lowest energy utilization rate in the cement production. In cement production, in order to improve grinding efficiency, reduce mill power consumption and improve cement quality, a small amount of grinding aid is usually added in the grinding process to reduce material surface energy in the grinding process, eliminate static electricity among material micro-powder particles and improve material fluidity in a mill, so that the grinding efficiency is improved and the cement particle gradation is improved.
The existing grinding aid is generally prepared by compounding triethanolamine, triisopropanolamine, diethanolisopropanolamine, glycerol, various chloride salts and the like. The above prior art solutions have the following drawbacks: triethanolamine, triisopropanolamine, diethanolisopropanolamine and the like are expensive, so that the cost of the grinding aid is greatly increased; the chloride ions in the chloride salt make the cement easily corrode the reinforcing steel bars in use and even affect the life of the building, so that the improvement is still left.
Disclosure of Invention
The invention aims to provide a low-cost and high-efficiency chlorine-free cement grinding aid and a preparation method thereof, and aims to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a low-cost high-efficiency chlorine-free cement grinding aid comprises the following components in parts by mass: 15-20 parts of compound reinforcing agent II type, 8-10 parts of sodium acetate and 12-15 parts of molasses.
The invention also provides a preparation method of the low-cost high-efficiency chlorine-free cement grinding aid, which comprises the following steps:
s1, preparing a composite reinforcing agent type II;
s2, adding molasses and a composite reinforcing agent type II into a reaction vessel, and stirring and mixing uniformly to form a premix;
s3, adding sodium acetate into the premix, stirring and mixing uniformly, and adding water until the sodium acetate is completely dissolved.
Preferably, the preparation of the composite reinforcing agent type II in the step S1 comprises the following steps:
s1a, hydrolysis reaction, namely mixing, heating and stirring quantitative methanesulfonic acid solution, dilute sulfuric acid and epoxy chloropropane in a hydrolysis reaction kettle for many times;
s1b, performing ammoniation reaction, namely pumping 3-chloro-1, 2-propanediol into an ammoniation reaction kettle, then adding ammonia water with the mass percentage concentration of 25% and ammoniation catalyst solution, and heating while stirring;
s1c, distilling, namely transferring the mixed solution in the two steps into a distillation kettle for distillation;
s1d, rectifying, namely transferring the liquid treated in the step S1c into a rectifying still for rectifying.
Preferably, in the step S1a, the epichlorohydrin is pumped into a glass lining hydrolysis reaction kettle with a stirring function and a mechanical seal function, then a small amount of methanesulfonic acid aqueous solution and a small amount of dilute sulfuric acid solution are respectively added into the hydrolysis reaction kettle, the temperature is controlled to be 58-62 ℃ by adopting a stirring and heating method, after stirring for 30min, the residual methanesulfonic acid aqueous solution is dripped, the reaction temperature during dripping is controlled to be 80-85 ℃, the dripping completion time is 1.5h, then the residual dilute sulfuric acid solution is dripped, the reaction temperature during dripping is controlled to be 100-105 ℃, the dripping completion time is 2.5h, and the hydrolysis reaction is completed.
Preferably, the ammoniation catalyst solution in the ammoniation reaction in step S1b is a liquid in which the ammoniation catalyst and hot ethanol are sufficiently dissolved.
Preferably, in the distillation process of step S1c, after the material is transferred to the distillation still, jacket steam of the distillation still is started to heat, ammonia water is recovered by atmospheric distillation, low-concentration ammonia water in the receiving tank is used for preparing ammonia water with a concentration of 25-27%, then the temperature of the material in the distillation still is cooled to 55 ℃, solids are separated out from the distillation still, then the material in the distillation still is transferred to a centrifuge for centrifugal separation, the solids are collected and post-treated, and the centrifugate enters the next step.
Preferably, in the rectification process of step S1d, after the material is transferred to the rectification kettle, the rectification kettle jacket is opened to heat and raise the temperature, the roots vacuum pump unit is opened at the same time, the condensate with the vapor phase temperature of 125-132 ℃ enters the finished product receiving tank, the material in the front fraction receiving tank is re-rectified and reused in the next rectification, and the material in the finished product receiving tank is the composite reinforcing agent type ii.
Compared with the prior art, the invention has the beneficial effects that:
1. by adopting the composite reinforcing agent type II, the invention is beneficial to better improving the early strength of the cement and the later strength of the cement, is beneficial to better improving the grinding aiding effect and is beneficial to better controlling the water demand of the cement.
2. The cement grinding aid prepared by the preparation method disclosed by the invention is non-toxic and harmless in all components, and cannot influence the environment and human health; meanwhile, the grinding aid is free of chloride ions, so that the building is not affected, and expensive raw materials such as triethanolamine, triisopropanolamine, diethanolisopropanolamine and the like are not added in the preparation process, so that the cost of the grinding aid is greatly reduced.
Drawings
FIG. 1 is a process diagram of a preparation method of the chlorine-free cement grinding aid with low cost and high efficiency.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The invention provides a technical scheme that: a low-cost high-efficiency chlorine-free cement grinding aid comprises 15 parts of a composite reinforcing agent II type, 12 parts of molasses and 8 parts of sodium acetate.
A preparation method of a low-cost and high-efficiency chlorine-free cement grinding aid comprises the following steps:
s1, preparing a composite reinforcing agent type II;
s2, adding molasses and a composite reinforcing agent type II into a reaction vessel, and stirring and mixing uniformly to form a premix;
s3, adding sodium acetate into the premix, stirring and mixing uniformly, and adding water until the sodium acetate is completely dissolved.
The composite reinforcing agent II is realized by the following technical scheme:
(1) hydrolysis reaction
Preparing quantitative methanesulfonic acid solution; preparing quantitative dilute sulfuric acid; pumping epoxy chloropropane into a glass-lined hydrolysis reaction kettle with stirring and mechanical sealing, then respectively adding a certain amount of methanesulfonic acid aqueous solution and a certain amount of dilute sulfuric acid solution into the hydrolysis reaction kettle, adopting a heating method while stirring, controlling the temperature at 58 ℃, dropwise adding the rest methanesulfonic acid aqueous solution after stirring for 30min, controlling the reaction temperature at 80 ℃ during dropwise adding, controlling the dropwise adding completion time at 1.5h, then dropwise adding the rest dilute sulfuric acid solution, controlling the reaction temperature at 100 ℃ during dropwise adding, controlling the dropwise adding completion time at 2.5h, and finishing the hydrolysis reaction.
(2) Ammoniation reaction
Adding an ammoniation catalyst into quantitative hot ethanol, and fully dissolving; pumping 3-chloro-1, 2-propanediol into a stainless steel ammoniation reaction kettle with stirring and mechanical sealing, then adding 25% ammonia water by mass percentage and the prepared ammoniation catalyst into the ammoniation reaction kettle, and adopting a method of heating while stirring.
(3) Distillation
And (3) after the material is transferred into a distillation kettle, starting steam of a distillation kettle jacket to heat, recovering ammonia water by normal pressure distillation, and using low-concentration ammonia water in a receiving tank to prepare ammonia water with the concentration of 25-27% for use. And after the distillation is finished, cooling the material in the distillation kettle to 55 ℃, separating out solids in the distillation kettle, transferring the material in the distillation kettle into a centrifugal machine for centrifugal separation, collecting and post-treating the solids, and allowing the centrifugate to enter a stainless steel rectification kettle.
(4) Rectification
After the material is transferred into a rectifying still, starting steam of a jacket of the rectifying still to heat and raise the temperature, simultaneously starting a Roots vacuum pump unit, and feeding condensate with the gas phase temperature of 125-132 ℃ into a finished product receiving tank. And adding the material in the front fraction receiving tank for re-rectification for utilization during next rectification, wherein the material in the finished product receiving tank is the composite reinforcing agent type II.
Example two
The invention provides a technical scheme that: a low-cost high-efficiency chlorine-free cement grinding aid comprises 15 parts of a composite reinforcing agent II type, 14 parts of molasses and 9 parts of sodium acetate.
The invention provides a preparation method of a low-cost and high-efficiency chlorine-free cement grinding aid, which comprises the following steps:
s1, preparing a composite reinforcing agent type II;
s2, adding molasses and a composite reinforcing agent type II into a reaction vessel, and stirring and mixing uniformly to form a premix;
s3, adding sodium acetate into the premix, stirring and mixing uniformly, and adding water until the sodium acetate is completely dissolved.
The composite reinforcing agent II is realized by the following technical scheme:
(1) hydrolysis reaction
Preparing quantitative methanesulfonic acid solution; preparing quantitative dilute sulfuric acid; pumping epoxy chloropropane into a glass-lined hydrolysis reaction kettle with stirring and mechanical sealing, then respectively adding a certain amount of methanesulfonic acid aqueous solution and a certain amount of dilute sulfuric acid solution into the hydrolysis reaction kettle, adopting a heating method while stirring, controlling the temperature at 60 ℃, dropwise adding the rest methanesulfonic acid aqueous solution after stirring for 30min, controlling the reaction temperature at 80-85 ℃ during dropwise adding, controlling the dropwise adding completion time at 1.5h, then dropwise adding the rest dilute sulfuric acid solution, controlling the reaction temperature at 101 ℃ during dropwise adding, controlling the dropwise adding completion time at 2.5h, and finishing the hydrolysis reaction.
(2) Ammoniation reaction
Adding an ammoniation catalyst into quantitative hot ethanol, and fully dissolving; pumping 3-chloro-1, 2-propanediol into a stainless steel ammoniation reaction kettle with stirring and mechanical sealing, then adding 25% ammonia water by mass percentage and the prepared ammoniation catalyst into the ammoniation reaction kettle, and adopting a method of heating while stirring.
(3) Distillation
And (3) after the material is transferred into a distillation kettle, starting steam of a distillation kettle jacket to heat, recovering ammonia water by normal pressure distillation, and using low-concentration ammonia water in a receiving tank to prepare ammonia water with the concentration of 25-27% for use. And after the distillation is finished, cooling the material in the distillation kettle to 55 ℃, separating out solids in the distillation kettle, transferring the material in the distillation kettle into a centrifugal machine for centrifugal separation, collecting and post-treating the solids, and allowing the centrifugate to enter a stainless steel rectification kettle.
(4) Rectification
After the material is transferred into a rectifying still, starting steam of a jacket of the rectifying still to heat and raise the temperature, simultaneously starting a Roots vacuum pump unit, and feeding condensate with the gas phase temperature of 125-132 ℃ into a finished product receiving tank. The material in the front fraction receiving tank is added for re-rectification and utilization during the next rectification, and the material in the finished product receiving tank is the composite reinforcing agent type II.
EXAMPLE III
The invention provides a technical scheme that: a low-cost high-efficiency chlorine-free cement grinding aid comprises 15 parts of a composite reinforcing agent II type, 15 parts of molasses and 10 parts of sodium acetate.
A preparation method of a low-cost and high-efficiency chlorine-free cement grinding aid comprises the following steps:
s1, preparing a composite reinforcing agent type II;
s2, adding molasses and a composite reinforcing agent type II into a reaction vessel, and stirring and mixing uniformly to form a premix;
s3, adding sodium acetate into the premix, stirring and mixing uniformly, and adding water until the sodium acetate is completely dissolved.
The composite reinforcing agent II is realized by the following technical scheme:
(1) hydrolysis reaction
Preparing quantitative methanesulfonic acid solution; preparing quantitative dilute sulfuric acid; pumping epoxy chloropropane into a glass-lined hydrolysis reaction kettle with stirring and mechanical sealing, then respectively adding a certain amount of methanesulfonic acid aqueous solution and a certain amount of dilute sulfuric acid solution into the hydrolysis reaction kettle, adopting a heating method while stirring, controlling the temperature at 62 ℃, dropwise adding the rest methanesulfonic acid aqueous solution after stirring for 30min, controlling the reaction temperature at 85 ℃ during dropwise adding, controlling the dropwise adding completion time to be 1.5h, then dropwise adding the rest dilute sulfuric acid solution, controlling the reaction temperature at 105 ℃ during dropwise adding, controlling the dropwise adding completion time to be 2.5h, and finishing the hydrolysis reaction.
(2) Ammoniation reaction
Adding an ammoniation catalyst into quantitative hot ethanol, and fully dissolving; pumping 3-chloro-1, 2-propanediol into a stainless steel ammoniation reaction kettle with stirring and mechanical sealing, then adding 25% ammonia water by mass percentage and the prepared ammoniation catalyst into the ammoniation reaction kettle, and adopting a method of heating while stirring.
(3) Distillation
And (3) after the material is transferred into a distillation kettle, starting steam of a distillation kettle jacket to heat, recovering ammonia water by normal pressure distillation, and using low-concentration ammonia water in a receiving tank to prepare ammonia water with the concentration of 25-27% for use. And after the distillation is finished, cooling the material in the distillation kettle to 55 ℃, separating out solids in the distillation kettle, transferring the material in the distillation kettle into a centrifugal machine for centrifugal separation, collecting and post-treating the solids, and allowing the centrifugate to enter a stainless steel rectification kettle.
(4) Rectification
After the material is transferred into a rectifying still, starting steam of a jacket of the rectifying still to heat and raise the temperature, simultaneously starting a Roots vacuum pump unit, and feeding condensate with the gas phase temperature of 125-132 ℃ into a finished product receiving tank. The material in the front fraction receiving tank is added for re-rectification and utilization during the next rectification, and the material in the finished product receiving tank is the composite reinforcing agent type II.
Comparative example
A cement sample containing the chlorine-free cement grinding aid is subjected to an experiment, and cement is prepared according to the proportion of 78% of clinker, 5% of desulfurized gypsum, 10% of fly ash and 7% of limestone in the experiment. The cement clinker, gypsum and limestone are crushed by a jaw crusher, and then all the components are uniformly mixed according to a proportion.
The cement grinding aid formulation is as follows.
The formula of No. I0.1 percent grinding aid is as follows: 15 percent of compound reinforcing agent II type, 12 percent of molasses and 8 percent of sodium acetate.
The formula of No. II 0.1 percent grinding aid is as follows: 15 parts of composite reinforcing agent II type, 14 parts of molasses and 9 parts of sodium acetate.
The formula of the No. III 0.1 percent grinding aid is as follows: 15 percent of compound reinforcing agent II type, 15 percent of molasses and 10 percent of sodium acetate.
The formula of the 0.1 percent grinding aid of IV number is as follows: 18 percent of compound reinforcing agent II type, 12 percent of molasses and 8 percent of sodium acetate.
The formula of 0.1 percent grinding aid V is as follows: 18 percent of compound reinforcing agent II type, 14 percent of molasses and 9 percent of sodium acetate.
VI, 0.1 percent of grinding aid formula is as follows: 18 percent of compound reinforcing agent II type, 15 percent of molasses and 10 percent of sodium formate.
No. VII 0.1% grinding aid formulation was: 20 percent of compound reinforcing agent II type, 12 percent of molasses and 8 percent of sodium acetate.
The formula of 0.1 percent grinding aid of No. VIII is as follows: 20 percent of compound reinforcing agent II type, 14 percent of molasses and 9 percent of sodium acetate.
The formula of 0.1 percent grinding aid of IX is as follows: 20 percent of compound reinforcing agent II type, 15 percent of molasses and 10 percent of sodium acetate.
Then respectively doping 0.1 percent grinding aid I-IX to prepare a cement sample, adding the cement sample into an experimental mill for milling for 30 minutes, and respectively measuring the 45 mu m sieve residue and the 80 mu m sieve residue of the milled cement sample according to GB/T1345-2005 'sieve analysis method for cement fineness inspection method'; and respectively measuring the 3d compressive strength (MPa) and the 28d compressive strength (MPa) and the 3d flexural strength (MPa) and the 28d compressive strength (MPa) of the ground cement sample according to GB/T17671-1999 cement mortar strength test method, wherein the experimental data refer to the following table 1:
table 1: comparison table of grinding aid and blank sample in each proportion
The following results can be obtained according to the data comparison in table 1:
1. the compound intensifier II can greatly improve the 3-day strength and the 28-day strength of the cement under the synergistic action of molasses and sodium acetate.
2. The composite reinforcing agent II has low cost, and can greatly reduce the cost of the grinding aid.
3. As the addition amount of the composite reinforcing agent type II is increased, the 3-day strength and the 28-day strength of the cement are firstly increased and then reduced, and the optimal addition amount is 18 percent.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The low-cost and high-efficiency chlorine-free cement grinding aid is characterized by comprising the following components in parts by mass: 15-20 parts of compound reinforcing agent II, 8-10 parts of sodium acetate and 12-15 parts of molasses.
2. The method for preparing the low-cost and high-efficiency chlorine-free cement grinding aid according to claim 1, which is characterized by comprising the following steps:
s1, preparing a composite reinforcing agent type II;
s2, adding molasses and the composite reinforcer II into the reaction vessel, and stirring and mixing uniformly to form a premix;
s3, adding sodium acetate into the premix, stirring and mixing uniformly, and adding water until the sodium acetate is completely dissolved.
3. The preparation method of the low-cost and high-efficiency chlorine-free cement grinding aid according to claim 2, characterized in that: the preparation steps of the composite reinforcing agent type II in the step S1 are as follows:
s1a, hydrolysis reaction, namely mixing, heating and stirring quantitative methanesulfonic acid solution, dilute sulfuric acid and epoxy chloropropane for many times in a hydrolysis reaction kettle;
s1b, performing ammoniation reaction, namely pumping 3-chloro-1, 2-propanediol into an ammoniation reaction kettle, then adding ammonia water with the mass percentage concentration of 25% and ammoniation catalyst solution, and heating while stirring;
s1c, distilling, namely transferring the mixed solution in the two steps into a distillation kettle for distillation;
s1d, rectifying, namely transferring the liquid treated in the step S1c into a rectifying still for rectifying.
4. The preparation method of the low-cost high-efficiency chlorine-free cement grinding aid according to claim 3, characterized in that: in the step S1a, epoxy chloropropane is pumped into a glass lining hydrolysis reaction kettle with stirring and mechanical sealing, then a small amount of methanesulfonic acid aqueous solution and a small amount of dilute sulfuric acid solution are respectively added into the hydrolysis reaction kettle, a stirring and heating method is adopted, the temperature is controlled to be 58-62 ℃, after stirring for 30min, the residual methanesulfonic acid aqueous solution is dripped, the reaction temperature during dripping is controlled to be 80-85 ℃, the dripping completion time is 1.5h, then the residual dilute sulfuric acid solution is dripped, the reaction temperature during dripping is controlled to be 100-105 ℃, the dripping completion time is 2.5h, and the hydrolysis reaction is finished.
5. The preparation method of the low-cost high-efficiency chlorine-free cement grinding aid according to claim 3, characterized in that: the ammoniation catalyst solution in the ammoniation reaction in the step S1b is a liquid in which the ammoniation catalyst and hot ethanol are fully dissolved.
6. The preparation method of the low-cost high-efficiency chlorine-free cement grinding aid according to claim 3, characterized in that: in the distillation process of the step S1c, after the material is transferred to a distillation kettle, the distillation kettle is started to jacket steam for heating, ammonia water is recovered by normal pressure distillation, low-concentration ammonia water in a receiving tank is used for preparing ammonia water with the concentration of 25-27%, then the temperature of the material in the distillation kettle is cooled to 55 ℃, solid is separated out from the distillation kettle, then the material in the distillation kettle is transferred to a centrifugal machine for centrifugal separation, the solid material is collected and post-treated, and the centrifugal liquid enters the next step.
7. The preparation method of the low-cost high-efficiency chlorine-free cement grinding aid according to claim 3, characterized in that: in the rectification process of the step S1d, after the material is transferred into a rectification kettle, the jacket steam of the rectification kettle is started to heat and raise the temperature, meanwhile, a Roots vacuum pump unit is started, condensate with the gas phase temperature of 125-132 ℃ enters a finished product receiving tank, the material in the front fraction receiving tank is added for rectification again during the next rectification, and the material in the finished product receiving tank is the composite reinforcing agent type II.
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| CN112408849A (en) * | 2020-11-03 | 2021-02-26 | 山东莒县江山科技有限公司 | Cement grinding aid and preparation method thereof |
| CN113979662A (en) * | 2021-12-02 | 2022-01-28 | 四川奥克化学有限公司 | Cement grinding aid and preparation method thereof |
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2022
- 2022-04-14 CN CN202210391627.9A patent/CN114890706A/en active Pending
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|---|---|---|---|---|
| US4204877A (en) * | 1979-01-15 | 1980-05-27 | Westvaco Corporation | Cement grinding aid and set retarder |
| KR101135598B1 (en) * | 2011-03-24 | 2012-04-17 | 노재호 | Compositions of grinding aids for the improving of grinding cement clinkers |
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