CN109279803B - Improvement of naphthalene series water reducing agent preparation method and control method of quality index thereof - Google Patents
Improvement of naphthalene series water reducing agent preparation method and control method of quality index thereof Download PDFInfo
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- CN109279803B CN109279803B CN201811466506.6A CN201811466506A CN109279803B CN 109279803 B CN109279803 B CN 109279803B CN 201811466506 A CN201811466506 A CN 201811466506A CN 109279803 B CN109279803 B CN 109279803B
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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
- C04B24/20—Sulfonated aromatic compounds
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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 relates to an improvement of a preparation method of a naphthalene water reducer, which comprises the following steps of 1) putting industrial naphthalene into a sulfonation device to obtain a sulfonated substance; 2) hydrolysis: transferring the sulfonated substance obtained in the step 1) into a condensation device for hydrolysis reaction; 3) condensation: dripping 37% of formaldehyde into the sulfonated substance obtained in the step 2), adding 600-750L of warm water at 50-90 ℃ to adjust the viscosity of the material when the material is viscous and when the current of a stirring motor rises by 9A, and continuing to keep the temperature until the material is viscous to obtain a condensed material; 4) neutralizing: adding 1250L of water into the condensed material obtained in the step 3) to perform dilution and neutralization reaction to obtain the liquid naphthalene water reducer. According to the preparation method of the naphthalene water reducer, the fixed water consumption is added in the condensation reaction process of preparing the naphthalene water reducer every time, and the current value of the stirring motor is used as a condensation control point, so that the molecular weight of the naphthalene water reducer prepared every time is consistent, and the process capability of producing the naphthalene water reducer is greatly improved.
Description
Technical Field
The invention relates to the technical field of concrete admixture preparation, in particular to an improvement of a naphthalene water reducer preparation method, and further provides a control method for judging the quality index of a naphthalene water reducer through a process capability index.
Background
The naphthalene water reducer is one of water reducers which are widely used in China, and the market share is about more than 30%. The naphthalene water reducer has mature production process and application technology, has more predictability particularly for excessive use than other water reducers, has better adaptability to powder-containing and mud-containing gravels, and can exert unique advantages particularly under the condition of complicated ground materials.
For example, the patent of the invention of a preparation method of a naphthalene water reducer, which is announced by the intellectual property office in 2017, 10 and 20 months, and the publication number of the patent is CN105236798B, discloses the production process steps of the naphthalene water reducer, and comprises the following steps:
(1) sulfonation of
Putting the methylnaphthalene in a molten state into a sulfonation device, heating to 110-140 ℃, slowly dropwise adding 98% concentrated sulfuric acid or fuming sulfuric acid, controlling the dropwise adding time to be more than 30min, keeping the temperature at 140-170 ℃ for sulfonation reaction for 2.5-3 h, and controlling the acidity of the feed liquid to be 18-40% at the end of the reaction to obtain a sulfonated methylnaphthalene material; the mass ratio of the methylnaphthalene to the sulfuric acid is 1: 1-2; putting phenol into a reactor after liquefaction, heating to 60-70 ℃, slowly dropwise adding 98% concentrated sulfuric acid or fuming sulfuric acid within 30min, controlling the temperature not to exceed 80 ℃, heating to 90-100 ℃ after dropwise adding, carrying out heat preservation reaction for 2-3 h, and controlling the acidity of the feed liquid to be 22-40% at the end point of the reaction to obtain a p-hydroxybenzene sulfonic acid material; the mass ratio of phenol to sulfuric acid is 1: 1-2;
(2) hydrolysis
Transferring the sulfonated methylnaphthalene material obtained in the step (1) into a hydrolysis naphthalene removal device, reducing the temperature to 100-130 ℃, adding water to control the acidity of the material liquid to be 10-32%, carrying out hydrolysis reaction for 15-30 min, removing unreacted methylnaphthalene along with water vapor azeotropy, and allowing the rest sulfonated methylnaphthalene material to enter the reaction in the step (3); cooling the azeotropic material to below 100 deg.c, standing for demixing and recovering methyl naphthalene in the lower layer for re-production;
(3) condensation of
Cooling the sulfonated methylnaphthalene material obtained in the step (2) to 90-95 ℃, mixing the sulfonated methylnaphthalene material with the p-hydroxybenzene sulfonic acid material obtained in the step (1) according to a certain proportion, transferring the mixture into a condensation device, adding water to adjust the acidity of a reaction system to be 20-25%, slowly dropwise adding formaldehyde acidified by concentrated sulfuric acid within 1-2 h, heating to 95-105 ℃ after dropwise adding, preserving heat, condensing for 3-4 h, and optionally adding water to adjust the viscosity of the material to obtain a condensed material; the mass ratio of the sulfonated methylnaphthalene to the p-hydroxybenzene sulfonic acid is 1.4-2: 1; the amount ratio of the formaldehyde to the p-hydroxybenzene sulfonic acid substance is 1.5-6: 1; the formaldehyde acidified by the concentrated sulfuric acid is obtained by adjusting the pH of a formaldehyde solution to 2-3 by the concentrated sulfuric acid and uniformly stirring;
(4) neutralization
And (4) transferring the condensation material obtained in the step (3) into a neutralization device, adding alkali liquor at the temperature of 60-80 ℃ for neutralization reaction until the pH value is 7.5-9, obtaining a liquid naphthalene water reducer after the reaction is finished, and further drying to obtain the naphthalene water reducer.
The third step of the existing steps for producing the naphthalene water reducer, namely condensation reaction, adopts time control to obtain a condensation material after the condensation reaction, but in the condensation reaction process, due to different gradients of temperature changes and inconsistent operation methods of operators when formaldehyde is dripped, the reaction speed in the condensation reaction process cannot be consistent, and when the material is viscous, a water adding method is adopted to reduce the viscosity of the material so as to ensure that the time parameter of the condensation meets the technological requirements. Although the time for controlling the condensation reaction is the same in the condensation reaction process for producing the naphthalene water reducer in the prior art, the concentration of the obtained condensation compound or condensation material can cause different viscosities of the condensation compound or condensation material of the condensation reaction due to the fact that the water consumption for hydrolysis is different in the midway water addition of the condensation reaction, and finally the product quality cannot be guaranteed due to the fact that the molecular weight of the produced naphthalene water reducer is different; the capability of the production process for producing the naphthalene water reducer is not enough to meet the quality standard requirement of the naphthalene water reducer product, and the quality index of the naphthalene water reducer cannot be stable. Whether the existing process for producing the product is stable or not is judged by a process capability index. The method for detecting the process capability of the process for producing the naphthalene water reducer is to perform a fluidity test on a detected product by adopting the water consumption of a reference sample of the naphthalene water reducer, detect the fluidity of the product, calculate the CPK value of the fluidity of the product so as to judge the process capability for producing the naphthalene water reducer, and control the quality of the naphthalene water reducer from the condition that the process capability for producing the naphthalene water reducer reaches the standard. The process capability index (CPK) refers to the degree of process capability meeting the product quality standard requirements (specification range, etc.), and is also called a process capability index, which refers to the actual processing capability of a process in a controlled state (stable state) within a certain time. It is the inherent ability of the process, or the ability of the process to ensure quality; the working procedure refers to a process in which five basic quality factors such as operators, machines, raw materials, process methods and production environments are combined, namely a production process of product quality.
The quality of the naphthalene water reducing agent depends on the size of the molecular weight of the naphthalene sulfonic acid formaldehyde condensate and the normal distribution of the molecular weight, the size of the molecular weight is directly reflected in the size of the viscosity of the naphthalene sulfonic acid formaldehyde condensate, and the molecular weight of the naphthalene sulfonic acid formaldehyde condensate is in direct proportion to the viscosity value under the same temperature and concentration condition.
Therefore, it is necessary to provide an improvement of the preparation method of the naphthalene water reducer to solve the defects of the prior art.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an improvement of a preparation method of a naphthalene water reducer, the preparation method of the naphthalene water reducer realizes condensation reaction by adding fixed water consumption in the condensation reaction process and taking the current value in the condensation reaction process as a condensation control point to obtain a condensation compound, the preparation method improves the process capability of producing the naphthalene water reducer, the CPK value of the process capability index reaches above B-level standard, namely the CPK value is not less than 1.0, and thus the quality of the produced naphthalene water reducer product is ensured.
The technical scheme of the invention is as follows:
the improvement of a preparation method of a naphthalene water reducer comprises the following steps:
1) sulfonation: putting industrial naphthalene in a sulfonation device, heating to 110-140 ℃, adding 98% concentrated sulfuric acid, and carrying out sulfonation reaction for 2.5-3.5 h at the temperature of 155-165 ℃ to obtain a sulfonated substance:
2) hydrolysis: transferring the sulfonated substance obtained in the step 1) into a condensation device, reducing the temperature to 110-120 ℃, adding 250-400L of hydrolysis water, and stirring for 10 minutes at the temperature to perform hydrolysis reaction;
3) condensation: cooling the sulfonated substance obtained in the step 2) to 93-97 ℃, slowly dripping 37% of formaldehyde within 1.5-2 h, and controlling the temperature to be 107-113 ℃ in the dripping process; after the dropwise adding, automatically heating to 115-118 ℃, preserving heat, when the material is viscous, namely the current of a stirring motor rises by 9A, adding 600-750L of warm water at 50-90 ℃ to adjust the viscosity of the material, and then continuously preserving heat until the material is viscous to obtain a condensed material; wherein the molar ratio of formaldehyde to naphthalene is 0.9-1.05: 1;
4) neutralizing: adding 1250L of water into the condensed material obtained in the step 3), diluting, transferring into a neutralization device, adding 30-32% liquid alkali liquor at the temperature of below 95 ℃, carrying out neutralization reaction until the pH value is 7-9, and obtaining the liquid naphthalene water reducer after the reaction is finished.
Preferably, in the step 1), the industrial naphthalene is placed in a sulfonation device, the temperature is raised to 130 ℃, sulfuric acid is added, and then the sulfonation reaction is carried out for 3 hours at 160 ℃ under the condition of heat preservation, so as to obtain a sulfonated substance. Wherein the sulfonate is alpha naphthalene sulfonic acid and beta naphthalene sulfonic acid.
Preferably, in step 2), 320L of water is added to perform the hydrolysis reaction. Wherein the hydrolysis reaction in step 2) is to hydrolyze off the sulfonic acid group in the alpha naphthalene sulfonic acid in the sulfonate.
Preferably, in step 3), 700L of warm water is added to dilute the material.
Based on the improvement of the preparation method of the naphthalene water reducer, the invention also provides a control method of the quality index of the naphthalene water reducer, which comprises the following steps:
(1) fluidity: carrying out fluidity test on the naphthalene water reducer obtained in the step 4) by using a cement paste fluidity tester to obtain the detected fluidity;
(2) fluidity index value: converting the detected fluidity in the step (1) and the fluidity of the standard sample to obtain a fluidity index value;
(3) calculating the Cpk value of the technological process capacity of the naphthalene series water reducing agent through the process capacity index CP;
(4) and judging the technological process capacity of the naphthalene water reducer according to the Cpk value so as to obtain whether the quality of the prepared naphthalene water reducer is stable.
In the step (1), the converted solid content of the naphthalene water reducer is 0.75% of the mass of the cement. Wherein the water cement ratio W/C is 0.29, and the cement is preferably the cement of conch P0.42.5.
In step (2), the fluidity index value is the test fluidity/standard fluidity.
In step (3), the process capability index Cp is the fluctuation state inherent to the characterization process, i.e. the technology level; the process capability index Cp is the situation where the mean value μ in the process coincides with the target value M. Wherein the content of the first and second substances,
Cp＝(Usl-Lsl)/6σ
Cpk＝(1-K)*Cp＝(1-2|M-μ|/T)*T/6σ＝T/6σ-|M-μ|/3σ
K＝|M-μ|/(T/2)＝2|M-μ|/T
T＝Usl-Lsl
σ is a standard deviation, Usl is an upper limit value of the specification value, and Lsl is a lower limit value of the specification value.
The invention has the beneficial effects that: compared with the prior art, the improvement of the preparation method of the naphthalene water reducer is that the fixed water consumption is added in the condensation reaction process when the naphthalene water reducer product is prepared every time, and the current value of the stirring motor in the condensation reaction process is used as a condensation control point, so that the molecular weight of the naphthalene water reducer product prepared every time is consistent, and the process capability of the naphthalene water reducer production is greatly improved on the premise that the product meets the quality standard.
Description of the drawings:
FIG. 1 is a test value of net slurry fluidity of a naphthalene series water reducer obtained by a conventional preparation method.
FIG. 2 is a test value of net slurry fluidity of a naphthalene water reducer prepared in a first modification example of the preparation method of the naphthalene water reducer.
FIG. 3 is a test value of net slurry fluidity of a naphthalene water reducer prepared in a second modification example of the preparation method of a naphthalene water reducer according to the present invention.
FIG. 4 is a test value of net slurry fluidity of a naphthalene water reducer prepared in a third modified example of the preparation method of the naphthalene water reducer.
Detailed Description
In order to make the object, technical solution and technical effect of the present invention more apparent, the present invention will be further described with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The improvement of a preparation method of a naphthalene water reducer comprises the following steps:
1) sulfonation: putting industrial naphthalene in a sulfonation device, heating to 110-140 ℃, adding sulfuric acid, and carrying out sulfonation reaction for 2.5-3.5 h at the temperature of 155-165 ℃ to obtain sulfonated substances of alpha naphthalene sulfonic acid and beta naphthalene sulfonic acid;
2) hydrolysis: transferring the sulfonated substance obtained in the step 1) into a condensation device, reducing the temperature to 110-120 ℃, adding 250-400L of hydrolysis water, and stirring for 10 minutes at the temperature to perform hydrolysis reaction.
3) Condensation: cooling the sulfonated substance obtained in the step 2) to 93-97 ℃, slowly dripping 37% of formaldehyde within 1.5-2 h, and controlling the temperature to be 107-113 ℃ in the dripping process; automatically heating to 115-118 ℃ after the dropwise adding is finished, when the material is viscous, increasing the current of a stirring motor by 9A, adding 600-750L of warm water at 50-90 ℃ to adjust the viscosity of the material, and then continuously preserving the heat until the material is viscous to obtain a condensed material;
4) neutralizing: adding 1250L of water into the condensed material obtained in the step 3), diluting, transferring into a neutralization device, adding 30-32% liquid alkali liquor at the temperature of below 95 ℃, carrying out neutralization reaction until the pH value is 7-9, and obtaining the liquid naphthalene water reducer after the reaction is finished.
Wherein the hydrolysis reaction in step 2) is to hydrolyze off the sulfonic acid group in the alpha naphthalene sulfonic acid in the sulfonate.
Based on the improvement of the preparation method of the naphthalene water reducer, the invention also provides a control method of the quality index of the naphthalene water reducer, which comprises the following steps:
(1) fluidity: carrying out fluidity test on the naphthalene water reducer obtained in the step 4) by using a cement paste fluidity tester to obtain the detected fluidity;
(2) fluidity index value: converting the detected fluidity in the step (1) and the fluidity of the standard sample to obtain a fluidity index value;
(3) calculating the Cpk value of the technological process capacity of the naphthalene series water reducing agent through the process capacity index CP;
(4) and judging the technological process capacity of the naphthalene series water reducing agent through the Cpk value.
The calculation formula of the fluidity index value is:
fluidity index value is detected fluidity/standard sample fluidity
In step (3), the process capability index Cp is the fluctuation state inherent to the characterization process, i.e. the technology level; the process capability index Cp is the situation where the mean value μ in the process coincides with the target value M. Wherein the content of the first and second substances,
Cp＝(Usl-Lsl)/6σ
Cpk＝(1-K)*Cp＝(1-2|M-μ|/T)*T/6σ＝T/6σ-|M-μ|/3σ
K＝|M-μ|/(T/2)＝2|M-μ|/T
T＝Usl-Lsl
σ is a standard deviation, Usl is an upper limit value of the specification value, and Lsl is a lower limit value of the specification value.
In the production process of the naphthalene water reducer, after the materials in the condensation device in the condensation reaction step are viscous, the torque of the stirring paddle in the condensation device is increased, and the current of the stirring motor of the condensation device is obviously increased. According to the working principle of the viscometer, the viscosity of materials is always the same at the same temperature, the same concentration and the same current value, and the molecular weight of the obtained product is also the same.
The following will further describe the improvement of the above-mentioned naphthalene water reducer preparation method with reference to specific examples.
Example one
Placing 1300Kg of industrial naphthalene in a sulfonation device, heating to 110 ℃, adding 1500Kg of 98% concentrated sulfuric acid, carrying out sulfonation reaction for 2.5h at 160-165 ℃ to obtain a sulfonated substance, transferring the sulfonated substance into a condensation device, adding 250L of water when the temperature is reduced to 110 ℃, stirring for 10 min at the temperature to carry out hydrolysis reaction to obtain a hydrolyzed sulfonated substance, starting to dropwise add 850Kg of 37% formaldehyde when the temperature of the sulfonated substance is reduced to 93 ℃, controlling the temperature within 107 ℃ in the process of dropwise adding the formaldehyde, keeping the dropwise adding time for 1.5-2 h, naturally heating to 115 ℃ after the dropwise adding is finished, continuing to keep the temperature at 115 ℃ until the material is viscous, increasing the current of a stirring motor by 9A, adding 380L of 68 ℃ warm water to adjust the viscosity of the material, continuing to keep the temperature until the current of the stirring motor increases by 9A again, adding tap water L to dilute the material, and transferring the diluted condensation material into a neutralization device for neutralization reaction, adding 1150Kg of alkali liquor with the concentration of 32% below 95 ℃ for neutralization reaction, and adjusting the pH value to 7-9 to obtain the liquid naphthalene water reducer.
Example two
1300Kg of industrial naphthalene is put into a sulfonating device, heated to 120 ℃, added with 1500Kg of 98 percent concentrated sulfuric acid, keeping the temperature at 160 ℃ for sulfonation reaction for 3h to obtain a sulfonated substance, transferring the sulfonated substance into a condensation device, cooling the temperature to 110 ℃, adding 400L of water, stirring for 10 min at the temperature for hydrolysis reaction to obtain hydrolyzed sulfonated substance, dropping 770Kg of 37% formaldehyde when the temperature of the material is reduced to 95 ℃, in the process of dripping formaldehyde, the temperature is controlled within 110 ℃, the dripping time is 1.5 hours, after the dripping is finished, the temperature is naturally raised to 115 ℃, and when the material is viscous by heat preservation and condensation at the temperature, namely, the current of the stirring motor is increased by 9A, 600L of 60-80 ℃ warm water is added, the temperature is kept at 115-117 ℃, when the material is viscous again, that is, the current of the stirring motor is increased by 9A, and 1250L of tap water is added to dilute the materials; and transferring the diluted material into a neutralization device for neutralization reaction, adding 1100Kg of 32% alkali liquor below 95 ℃, performing neutralization reaction, and adjusting the pH value to 7-9 to obtain the liquid naphthalene water reducer.
EXAMPLE III
1300Kg of industrial naphthalene is put into a sulfonating device, heated to 130 ℃, added with 1500Kg of 98 percent concentrated sulfuric acid, preserving the temperature at 165-166 ℃ for sulfonation reaction for 3h to obtain a sulfonated substance, transferring the sulfonated substance into a condensation device, cooling the temperature to 110 ℃, adding 320L of water, stirring for 10 min at the temperature for hydrolysis reaction to obtain hydrolyzed sulfonated substance, dropping 850Kg of 37% formaldehyde when the temperature of the material is reduced to 95 ℃, in the process of dripping formaldehyde, the temperature is controlled to be within 105 ℃, the dripping time is 1.5 hours, after the dripping is finished, the temperature is naturally raised to 115 ℃, and when the material is viscous by heat preservation and condensation at the temperature, that is, the current of the stirring motor is increased by 9A, 680L of warm water at 60-80 ℃ is added, the temperature is kept at 115-117 ℃, and when the material is viscous, that is, the current of the stirring motor is increased by 9A, and 1250L of tap water is added to dilute the materials; and transferring the diluted material into a neutralization device for neutralization reaction, adding 1050Kg of 32% alkali liquor at the temperature of below 95 ℃, performing neutralization reaction, and adjusting the pH value to 7-9 to obtain the liquid naphthalene water reducer.
The net slurry fluidity index of the naphthalene water reducer prepared in the above examples one to three and the prior art was tested. Specifically, the naphthalene water reducer is adopted, and the converted solid content is 0.75% of the mass of the cement. Wherein the water cement ratio W/C is 0.29, and the cement is preferably the cement of conch P0.42.5.
Table 1 shows Cpk values obtained by randomly extracting fluidity index values of 80 samples to be tested and calculating the fluidity index values of the naphthalene water reducer obtained under the condition of preparing the naphthalene water reducer according to the proportion in the background art.
As can be seen from the values in table 1 above, the following results were obtained by calculation: the alpha is 0.0446, the Cpk value is 0.1946<0.67, the process capability of the product production process is poor, and the product quality fluctuation of the naphthalene water reducing agent produced by the process is large, thereby bringing quality influence on the use of the product in concrete.
Table 2 shows Cpk values obtained by randomly extracting fluidity index values of 80 samples to be tested and calculating the fluidity index values of the naphthalene water reducing agent obtained under the condition of the example.
Table 3 shows Cpk values calculated by randomly extracting fluidity index values of 80 samples of the naphthalene water reducing agent obtained under the two conditions of the example.
Table 4 shows Cpk values obtained by randomly extracting fluidity index values of 80 samples to be tested and calculating the fluidity index values of the naphthalene water reducing agent obtained under the three conditions of the example.
As can be seen from the numerical values in tables 1 to 4, the net slurry fluidity process capability indexes of the naphthalene water reducers prepared in the first to third examples are all larger than 1, which indicates that the quality indexes and the stability of the naphthalene water reducers prepared in the first to third examples are superior to those of the naphthalene water reducers prepared in the prior art, wherein the water reducing effect and the quality stability of the naphthalene water reducers prepared in the third example are optimal, which means that the quality of the naphthalene water reducers prepared by the preparation method is optimal.
The improvement of the preparation method of the naphthalene water reducer is that a fixed water consumption is added in the condensation reaction process when a naphthalene water reducer product is prepared every time, the current value in the condensation reaction process is used as the viscosity in the condensation reaction, the molecular weight of the naphthalene water reducer product prepared every time is relatively consistent under the condition of not increasing the working difficulty and the cost, the quality of the naphthalene water reducer product prepared by the preparation method meets the quality standard, the process capability of the production of the naphthalene water reducer is improved, the quality of the produced naphthalene water reducer product is controlled, the quality of the product is improved, the yield of the produced product is improved, the naphthalene water reducer prepared by the method has good adaptability to various concretes, and the water reducing effect is good.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the present invention pertains, the architecture form can be flexible and varied without departing from the concept of the present invention, and a series of products can be derived. But rather a number of simple derivations or substitutions are made which are to be considered as falling within the scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of a naphthalene water reducer is characterized by comprising the following steps;
1) sulfonation: putting industrial naphthalene in a sulfonation device, heating to 110-140 ℃, adding 98% concentrated sulfuric acid, and carrying out sulfonation reaction for 2.5-3.5 hours at the temperature of 155-165 ℃ to obtain a sulfonated substance;
2) hydrolysis: transferring the sulfonated substance obtained in the step 1) into a condensation device, reducing the temperature to 110-120 ℃, adding 250-400L of hydrolysis water, and stirring for 10 minutes at the temperature to perform hydrolysis reaction;
3) condensation: cooling the sulfonated substance obtained in the step 2) to 93-97 ℃, slowly dripping 37% of formaldehyde within 1.5-2 h, and controlling the temperature to be 107-113 ℃ in the dripping process; after the dropwise adding, automatically heating to 115-118 ℃ for heat preservation, when the material is viscous, adding 600-750L of warm water at 50-90 ℃ to adjust the viscosity of the material when the current of a stirring motor rises by 9A, and then continuously preserving heat until the material is viscous to obtain a condensed material;
4) neutralizing: adding 1250L of water into the condensed material obtained in the step 3), diluting, transferring into a neutralization device, adding 30-32% liquid alkali liquor at the temperature of below 95 ℃, carrying out neutralization reaction until the pH value is 7-9, and obtaining the liquid naphthalene water reducer after the reaction is finished;
the method for controlling the quality index of the naphthalene water reducer prepared by the method comprises the following steps:
(1) fluidity: carrying out fluidity test on the naphthalene water reducer obtained in the step 4) by using a cement paste fluidity tester to obtain the detected fluidity;
(2) fluidity index value: converting the detected fluidity in the step (1) and the fluidity of the standard sample to obtain a fluidity index value;
(3) calculating the Cpk value of the technological process capacity of the naphthalene series water reducing agent through the process capacity index CP;
(4) and judging the technological process capacity of the naphthalene water reducer through the Cpk value so as to obtain the quality stability of the prepared naphthalene water reducer.
2. The preparation method of the naphthalene water reducer according to claim 1, wherein in the step 2), 320L of water is added for hydrolysis reaction.
3. The preparation method of the naphthalene water reducer according to claim 1, wherein in the step 3), the molar ratio of formaldehyde to naphthalene is 0.9-1.05: 1.
4. the method for preparing a naphthalene based water reducer according to claim 1, wherein in the step 1), the sulfonated compound is alpha naphthalene sulfonic acid and beta naphthalene sulfonic acid.
5. The method for preparing a naphthalene based water reducer according to claim 1, wherein the hydrolysis reaction in the step 2) is to hydrolyze off sulfonic acid groups in alpha naphthalene sulfonic acid in the sulfonate.
6. The method for preparing the naphthalene water reducer according to claim 1, wherein 700L of warm water at 70 ℃ is added to dilute the material in the step 3).
7. The method for controlling the quality index of the naphthalene water reducer obtained by the preparation method according to any one of claims 1 to 6, is characterized by comprising the following steps of:
(1) fluidity: carrying out fluidity test on the naphthalene water reducer obtained in the step 4) by using a cement paste fluidity tester to obtain the detected fluidity;
(2) fluidity index value: converting the detected fluidity in the step (1) and the fluidity of the standard sample to obtain a fluidity index value;
(3) calculating the Cpk value of the technological process capacity of the naphthalene series water reducing agent through the process capacity index CP;
(4) and judging the technological process capacity of the naphthalene water reducer through the Cpk value so as to obtain the quality stability of the prepared naphthalene water reducer.
8. The method for controlling the quality index of the naphthalene water reducer according to claim 7, wherein in the step (1), the converted solid content of the naphthalene water reducer is 0.75% of the mass of the cement.
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| CN110156368A (en) * | 2019-05-24 | 2019-08-23 | 莱芜市兆信新材料股份有限公司 | A kind of preparation method of gypsum water-reducing agent |
| CN111470793B (en) * | 2020-05-12 | 2022-03-04 | 广东柯杰科技实业有限公司 | High-dispersity high-quality naphthalene-based high-efficiency water reducing agent and preparation method thereof |
| CN111689879A (en) * | 2020-06-03 | 2020-09-22 | 浙江五龙新材股份有限公司 | Clean production method of dispersing agent |
| CN114106893A (en) * | 2021-12-24 | 2022-03-01 | 莱芜市兆信新材料股份有限公司 | Preparation method of naphthalene water reducer for coal water slurry |
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Denomination of invention: Improvement of preparation method of naphthalene water reducer and control method of its quality index Effective date of registration: 20211208 Granted publication date: 20210507 Pledgee: China Co. truction Bank Corp Huizhou Huiyang branch Pledgor: GUANGDONG KELONG ZHIGU NEW MATERIAL CO.,LTD. Registration number: Y2021980014349 |